INVESTIGATIONS IN FISH CONTROL

47. Preparation and Properties of Quinaldine Sulf ate, 

an Improved Fish Anesthetic

48. Toxicity of Quinaldine Sulfate to Fish

49. The Efficacy of Quinaldine Sulfate as an 

Anesthetic for Freshwater Fish

50. Residue of Quinaldine in Ten Species of Fish 

Following Anesthesia with Quinaldine Sulfate

United States Department of the Interior

Fish and Wildlife Service 

Bureau of Sport Fisheries and Wildlife
Investigations in Fish Control, published by the Bureau of Sport Fisheries and Wildlife, include reports on the results of work at the Bureau's Fish Control Laboratories at 

La Crosse, Wis., and Warm Springs, Ga., and reports of other studies related to that work. 

Though each report is regarded as a separate publication, several may be issued under a 

single cover, for economy.

Current reports in this series are 

(Reports 1 and 2 are in one cover.)

1. Laboratories and Methods for Screening Fish-Control Chemicals, by Robert E. Lennon and 

Charles R. Walker. 1964. 15 p.

2. Preliminary Observations on the Toxicity of Antimycin A to Fish and Other Aquatic

Animals, by Charles R. Walker, Robert E. Lennon, and Bernard L. Berger. 1964. 18 p.

(Reports 3 through 8 are in one cover.)

3. Minimum Lethal Levels of Toxaphene as a Piscicide in North Dakota Lakes, by Dale L. 

Henegar. 1966. 16 p.

4. Effects of Toxaphene on Plankton and Aquatic Invertebrates in North Dakota Lakes, by 

Robert G. Needham. 1966. 16 p.

5. Growth Rates of Yellow Perch in Two North Dakota Lakes After Population Reduction with 

Toxaphene, by Donald C. Warnick. 1966. 9 p.

6. Mortality of Some Species of Fish to Toxaphene at Three Temperatures, by Mahmoud Ahmed 

Mahdi. 1966. 10 p.

7. Treatment of East Bay, Alger County, Michigan, with Toxaphene for Control of Sea 

Lampreys, by William E. Gaylord and Bernard R. Smith. 1966. 7 p.

8. Effects of Toxaphene on Fishes and Bottom Fauna of Big Kitoi Creek, Afognak Island, 

Alaska, by William R. Meehan and William L. Sheridan. 1966. 9 p.

(Reports 9 through 11 are in one cover.)

9. Relation of Chemical Structure to Fish Toxicity in Nitrosalicylanilides and Related Compounds, by Charles R. Walker, Roland J. Starkey, and Leif L. Marking. 1966. 12 p.

10. Evaluation of p_,p_'-DDT as a Reference Toxicant in Bioassays, by Leif L. Marking.

1966. 10 p.

11. Evaluation of an Electronic Method of Measuring Hematocrits of Fish, by Richard A. 

Schoettger and Arnold M. Julin. 1966. 11 p.

(Reports 12 through 17 are in one cover.)

12. Toxicity of MS-222 to Selected Fishes, by Leif L. Marking. 1967. 10 p.

13. Efficacy of MS-222 as an Anesthetic on Four Salmonids, by Richard A. Schoettger and 

Arnold M. Julin. 1967. 15 p.

14. Method for Determining MS-222 Residues in Fish, by Charles R. Walker and Richard A. 

Schoettger. 1967. 10 p.

15. Residues of MS-222 in Four Salmonids Following Anesthesia, by Charles R. Walker and 

Richard A. Schoettger. 1967. 11 p.

16. Annotated Bibliography on MS-222, by Richard A. Schoettger. 1967. 15 p.

17. MS-222 as an Anesthetic for Channel Catfish: Its Toxicity, Efficacy, and Muscle Residues, 

by Richard A. Schoettger, Charles R. Walker, Leif L. Marking, and Arnold M. Julin.

1967. 14 p.

(Reports 18 through 21 are in one cover.)

18. Toxicity of 22 Therapeutic Compounds to Six Fishes, by Wayne A. Willford. 1967. 10 p.

19. Toxicity of Bayer 73 to Fish, by Leif L. Marking and James W. Hogan. 1967. 13 p.

20. Toxicity of Dimethyl Sulfoxide (DMSO) to Fish, by Wayne A. Willford. 1967. 8 p.

21. Labor-Saving Devices for Bioassay Laboratories, by Robert J. Hesselberg and Ralph M. 

Burress. 1967. 8 p.

Fish Control Laboratories

Bureau of Sport Fisheries and Wildlife

U.S. Department of the Interior

P.O. Box 862

La Crosse, Wisconsin 54601

Continued on inside back cover 
INVESTIGATIONS IN FISH CONTROL

47. Preparation and Properties of Quinaldine Sulfate,

an Improved Fish Anesthetic

By John L. Alien and Joe B. Sills

48. Toxicity of Quinaldine Sulfate to Fish

By Leif L. Marking and Verdel K. Dawson

49. The Efficacy of Quinaldine Sulfate as an 

Anesthetic for Freshwater Fish

By Philip A. Gilderhus, Bernard L. Berger, 

Joe B. Sills, and Paul D. Harman

50. Residue of Quinaldine in Ten Species of Fish 

Following Anesthesia with Quinaldine Sulfate

By Joe B. Sills, John L. Alien, Paul D. Harman, 

and Charles W. Luhning

United States Department of the Interior, Rogers C. B. Morton, Secretary

Nathaniel P. Reed, Assistant Secretary for 

Fish and Wildlife and Parks 

Fish and Wildlife Service

Bureau of Sport Fisheries and Wildlife, Spencer H. Smith, Director

Washington, D.C. April 1973
IN THIS COVER

Pages

Preparation and Properties of Quinaldine Sulfate, an Improved

Fish Anesthetic, by John L. Alien and Joe B. Sills......... 1-7

Toxicity of Quinaldine Sulfate to Fish, by Leif L. Marking

and Verdel K. Dawson. ........................... i_8

The Efficacy of Quinaldine Sulfate as an Anesthetic for Freshwater 

Fish, by Philip A. Gilderhus, Bernard L. Berger, Joe B. Sills, 

and Paul D. Harman............................. 1-9

Residue of Quinaldine in Ten Species of Fish Following

Anesthesia with Quinaldine Sulfate, by Joe B. Sills, John L. 

Alien, Paul D. Harman, and Charles W. Luhning ........

ii
FOREWORD

An anesthetic used on food and game fishes must bear a label registered 

by the U.S. Food and Drug Administration. The requirements for registration include data on the toxicity of the drug to exposed fish; on the efficacy 

as an anesthetic to selected fishes of several life stages in waters of different pH, hardness, and temperature; and on the residues of drug present 

in edible fish tissues following exposure. The following papers are concerned with results of registration-oriented research on toxicity, efficacy, 

and residues of quinaldine sulfate (QdSO^) when employed as an anesthetic 

for selected species of coldwater and warmwater fish. The data will be used 

to support a petition for registration of the anesthetic.

Chemists at the Fish Control Laboratories developed quinaldine sulfate as 

an improved formulation of quinaldine, a coal tar derivative used extensively 

in the manufacture of dyes, pharmaceuticals, and fine organic chemicals. 

Quinaldine came into use as a fish anesthetic in 1958 and is preferred in 

some fish culture and fishery management operations because of its low 

order of toxicity to fish in long exposures. Although effective and economical, the 95-percent quinaldine used is an oily liquid that is insoluble in water 

and possesses a strong, disagreeable odor. In addition to these disadvantages, 

the 5 percent of other quinones present would have to be identified and studied 

in detail before an attempt was made to obtain registration of quinaldine as a 

fish anesthetic.

In contrast, quinaldine sulfate is a pure, crystalline formulation that is 

water soluble, has little odor, is easy to handle, and is effective as a fish 

anesthetic. Its purity would be an advantage in seeking registration. Thus, 

we chose to do registration-oriented research on quinaldine sulfate rather 

than on quinaldine.

Robert E. Lennon, Director 

Fish Control Laboratories 

June 2, 1972

iii

INVESTIGATIONS IN FISH CONTROL

47. Preparation and Properties of Quinaldine Sulf ate, 

an Improved Fish Anesthetic

By John L. Alien and Joe B. Sills

United States Department of the Interior, Rogers C. B. Morton, Secretary

Nathaniel P. Reed, Assistant Secretary for 

Fish and Wildlife and Parks, 

Fish and Wildlife Service

Bureau of Sport Fisheries and Wildlife, Spencer H. Smith, Director

Washington, D.C. April 1973
CONTENTS

Page 

Abstract. ...................................... 3

Introduction. .................................... 3

Methods and Materials ............................. 3

Results. ....................................... 4

Discussion ..................................... 6

Conclusions. .................................... 6

References ..................................... 6
PREPARATION AND PROPERTIES OF QUINALDINE SULFATE, 

AN IMPROVED FISH ANESTHETIC

By John L. Alien and Joe B. Sills

Fish Control Laboratories, La Crosse, Wisconsin

and Warm Springs, Georgia

ABSTRACT. The preparation of quinaldine sulfate (QdSO4 ) from practical grade quinaldine and sulfuric acid yields a crystalline product which is 

water soluble and easily purified by recrystallization. The product conforms 

with the empirical formula CioHn NSO4 and assays 99.4 percent pure by 

titration. The crystalline material has little odor and is water soluble; thus, 

it is less objectionable and much easier to handle than quinaldine for anesthetizing fish.

INTRODUCTION

Quinaldine (2-methylquinoline) was suggested 

as an anesthetic for fish by Muench (1958) and has 

been used safely and effectively to facilitate general handling of fishes over a wide variety of conditions. This chemical presumably enters a fish's 

body by absorption across the gill membranes, but 

its specific physiological mode of action has not 

been determined. At a concentration of 10 mg/1, 

quinaldine has been shown by Clark and Granath 

(1968) to depress the frequency of electrical discharge of the gymnotid eel (Sternarchus albifrons). 

Trams and Brown (1970) using brain homogenates 

from nurse sharks (Ginglymostoma cirratum) 

and cow-nosed rays (Rhinoptera bonasus) have 

shown that 10~3 M quinaldine produced a 50- 

percent inhibition of acetylcholinesterase and 

butyrycholinesterase. However, Trams and 

Brown do not think this is the mode of action 

of quinaldine.

Practical grade quinaldine is an economical 

and effective tool; however, it is an oily liquid 

not readily soluble in water, and has a strong, 

disagreeable odor. Jodlbauer and Salvendi (1905) 

noted that quinoline and the sulfuric acid salt of 

quinoline both exhibited anesthetic properties 

with fish. Sills andHarman (1970) showed quinaldine sulfate possesses the same desirable ane;sthetic properties as quinaldine. The salt is a

crystalline form of the anesthetic with none of 

the unfavorable characteristics of the liquid, and 

is a product of high purity. The objectives of this 

paper are to present the preparation of the quinaldine salt and its chemical characterization as 

an improved formulation for use as an anesthetic 

by fishery workers.

METHODS AND MATERIALS

Since commercial sources of quinaldine sulfate 

could not be located, the quinaldine sulfate was 

prepared from Eastman Kodak, 95-percent quinaldine. Initially, two small batches of quinaldine 

sulfate were prepared by reacting 20 ml of quinaldine with 7.0 ml of concentrated sulfuric acid 

in the presence of a hydrocarbon solvent. Later, 

four batches of quinaldine sulfate (2-methylquinoline sulfate) were prepared using the following batch formula:

quinaldine, 500 grams or 3.49 moles 

sulfuric acid, 190 ml or 3.42 moles 

iso-octane, 500 ml.

The quinaldine and iso-octane were placed in 

a 4,000-ml reaction flask and were mixed thoroughly with a mechanical stirrer. The reaction 

mixture was placed in an ice bath, and concentrated sulfuric acid was added slowly while the
4 Investigations in Fish Control 47: Bureau of Sport Fisheries and Wildlife

mixture was stirred vigorously. The rate of sulfuric acid addition was adjusted to keep the temperature of the mixture below the boiling point of 

iso-octane (99.3° C.). The resultant mixture was 

filtered using vacuum, and the filter cake was 

washed with approximately 250 ml of benzene. 

The product was recrystallized from methanol. 

The recrystallization yielded approximately 

566 grams of a bright red crystalline material 

(68.5-percent yield).

RESULTS

The quinaldine sulfate was tested for purity 

and for structural changes as a result of the reaction of sulfuric acid with quinaldine. The recrystallized quinaldine sulfate was soluble in 

water and alcohol and insoluble in benzene and 

ether (table 1.). The melting range of the material 

was211°-214° C.Stecher et al. (1968)list the 

melting range of quinaldine sulfate as 211°- 

213° C. When titrated to a phenolphthalein end 

point with 0.1 N sodium hydroxide, the product 

was determined to be 99.4 percent C10 Hn NSO4 . 

The infrared spectra of practical grade quinaldine

TABLE I.- -The solubility of quinaldine sulfate in seven 

different solvents at 20° C.

Solvent Solubility 

(g/100 ml)

water

methyl alcohol

ethyl alcohol

acetone

ethyl ether

benzene

hexane

104.05 

7.44 

2.27 

0.08 

1 i 

i 

i

1 Insoluble = less than 0.01 grams dissolves in 100 ml 

of solvent.

and the free base of quinaldine sulfate were determined in carbon tetrachloride (from 4,000 1< 

1,300 cm-1 ) and in carbon disulfide (from 1,30C 

to 400 cm-1 ). The spectrum of free base of 

quinaldine sulfate shows all the absorption ban 

present in the spectrum of practical grade quir 

aldine(fig. 1). The infrared spectrum of quinaldine sulfate in a KBr pellet also contains bar 

at 1,000 and 1,170 cm" 1 indicating presence of 

sulfate and a broad band at 2,700 cm"1 which i 

dicates an amine salt. The ultraviolet spectrui 

of the product in 0.1 N H2 SO4 gives absorptic 

maxima at 236 and 317 nm (fig. 2).

An aqueous solution of quinaldine sulfate wa 

made alkaline and extracted with hexane to gi1 

a solution of the free base of quinaldine in 

hexane. The resulting hexane solution was injected into a gas chromatograph equipped with 

1 80 cm x 4 mm column packed with 5-percent 

carbowax20 M on gas chromQ 80/100 mesh i 

130° C. and a flow rate of 60 ml/minute. A 

single peak with the same retention time as qu 

aldine eluted after the solvent peak.

The product gives a positive test for sulfate 

using the USP XVII (1965) test for sulfates.

Two batches of quinaldine sulfate prepared 1 

the above method were subjected to elemental 

analysis 1 with the following results.

%C

Calculated 49.78 4.60 5.81 13.29 26,

Sample 1 

Sample 2

49.40 4.59

49.48 4.57

5.89

5.83

13.15 26.

13.39 26,

The elemental analysis indicates an empirical 

formula of C 10 HU NSO4 , which is the empiric

1 The elemental analysis was done by Galbraith Labc 

ratories, Inc., Knoxville, Tennessee.
Alien and Sills; Preparation and Properties of Quinaldine Sulfate

Schoettger, Richard A., and Arnold M. JuJin.

1969. The efficacy of quinaldine as an anesthetic for 

seven species of fish. U.S. Bureau of Sport Fisheries 

and Wildlife, Investigations in Fish Control No. 22, 

10 p.

Sills, Joe B.f and John L. Alien.

1971. The effect of pH on the efficacy and residues of 

quinaldine. Transactions of the American Fisheries Society, vol. 100, no. 3, p. 544-545.

Sills, Joe B., and Paul D. Harman.

1970. Efficacy and residues of quinaldine sulfate, an 

anesthetic for striped bass (Roccus saxatilis). Proceedings of 24th Annual Conference of the Southeastern Association of Game and Fish Commissioners, p.546-549.

Stecher, Paul G., M. Windholz, D. Leahy, D8 M0 Bolton, 

and L. G. Eaton.

1968. The Merck Index. Eighth edition. Merck and

Company Incorporated, Rahway, New Jersey.

1713 p.

Trams, Eberhard G., and Elise A. B. Brown.

1970. Metabolism of quinaldine (2-methylquinoline) 

uptake and excretion by nurse sharks. Life 

Sciences, vol. 9, part II. p. 27-35.

The United States Pharmacopeial Convention, Inc. 

meeting at Washington, D.C., March 29 and 30,1960. 

1965. The Pharmacopia of the United States of 

America. Seventeenth revision, 1156 p.
Investigations in Fish Control 47: Bureau of Sport Fisheries and Wildlife

0.6

0.5

0.4

u

c 

o 

.a

o 0.3

CO

0.2

0.

200 240 280 320 

Wavelength, nm

360

Figure 2.~=Ultraviolet spectrum of quinaldine sulfate 

in 0.1 N sulfuric acid.

formula of quinaldine sulfate given by Stecher 

etal. (1968). The product can be represented by 

the semi-structural formula given below.

H 2S04

DISCUSSION

The quinaldine sulfate prepared during this 

study has been shown to be a product o"f high 

purity. The reaction of sulfuric acid with quinaldine using the conditions of preparation we 

used in this investigation did not alter the structure of the quinaldine molecule. The sulfate salt 

of the nitrogenous base (quinaldine) was recovered in good yield (68.5 percent).

Schoettger and Julin (1969) indicated that quinaldine is inactive as an anesthetic for fish at pH 6

or below. Sills and Alien (1971) correlated the 

efficacy of quinaldine at a given pH with the ionization constant of the molecule. They indicated 

the uptake of the chemical by fish is dependent c 

the amount of the quinaldine present in thewatei 

in the lipophilic, free base form. Quinaldine sulfate is an acid salt and will depress the pH of ar 

esthetic solutions, particularly in soft water. Tt 

depression of pH can be overcome by buffering 

the anesthetic solutions.

CONCLUSIONS

1. Recrystallization of quinaldine sulfate prepared by the reaction of quinaldine with sulfuric acid gives a product of high purity.

2. Quinaldine sulfate is a water soluble crystalline material with little odor.

3. Since this salt is also an effective anesthetic 

it isv a more useful tool for fishery work tha 

practical grade quinaldine.

REFERENCES

Bell, Gordon R.

19670 A guide to the properties, characteristics, ai 

uses of some general anesthetics for fish. Fishe 

Research Board of Canada, Bulletin 148, 2nd edit 

revised, 11 p.

Clark, Warren L., and Louis P. Granath.

1968. Effect of drugs on the frequency of the electi 

output of Sternarchus albifrons. American Zoolo 

vol. 8, no. 4, p. 780.

Jodlbauer, A., and H. Salvendi.

1905. On the effects of acridine. Archives Internationales de Pharmacodynamie et de Therapie, vo] 

p. 224-236,

Klontz, George W.

1964. Anesthesia of fishes. Proceedings of the Syr 

posium on Experimental Animal Anesthesiology. 

Brooks Air Force Base, December 14=16, 13 p.

McFarland, William N.

1966. The use of anesthetics for the handling and tl 

transport of fishes. California Fish and Game, v 

46, no. 4, p. 407-431.

Muench, Bruce.

1958. Quinaldine, a new anesthetic for fish. Progr 

sive Fish-Culturist, vol. 20, no. 1, p. 42=44.
Alien and Sills: Preparation and Properties of Quinaldine Sulfate 5

100

50

0

100

50

100

50

4000 3500 3000 2500 2000 1800 1600 1400 1200 1000 800 600 4OO

Wavenumber cm- 1

rigure 1. Infrared spectra of Eastman Kodak practical grade quinaldine (top), and the free base of quinaldine 

sulfate middle) in carbon tetrachloride and carbon disulfide, and quinaldine sulfate (bottom) in a 

KBr pellet.

518-291 O - 73 - 2
INVESTIGATIONS IN FISH CONTROL

48. Toxicity of Quinaldine Sulfate to Fish

By Leif L. Marking and Verdel K. Dawson

United States Department of the Interior, Rogers C. B. Morton, Secretary

Nathaniel P. Reed, Assistant Secretary for 

Fish and Wildlife and Parks, 

Fish and Wildlife Service

Bureau of Sport Fisheries and Wildlife, Spencer H. Smith, Director

Washington, D.C. . April 1973
Contents

Page

Abstract................................................. 3

Introduction. .............................................. 3

Methods and Materials. ....................................... 3

Results. ................................................. 4

Effects of QdSO4 oa test solutions ............................. 4

Species and sizes of fish ................................... 4

Effects of temperature and water hardness....................... 4

Effects of buffered and aged solutions of QdSO4. ................... 5

Discussion ............................................... 7

Conclusions. .............................................. 7

References ............................................... 7
TOXICITY OF QUINALDINE SULFATE TO FISH

By Leif L. Marking and Verdel K. Dawson 

Fish Control Laboratories, La Crosse, Wisconsin

ABSTRACT.--The acute toxicities of the candidate fish anesthetic, quinaldine sulfate (QdSC>4), were determined against selected species of coldwater and warmwater fishes. The LC50's (concentrations producing 50- 

percent mortality) were derived for 3-, 6-, 24-, and 96-hour exposures in 

bioassays with different temperatures, hardnesses, and pH's. The 96-hour 

LC50's of QdSO4 ranged from 6.8 mg/1 for largemouth bass to 72.5 mg/1 for 

carp. In very soft water QdSO4 solutions are acidic and considerably less 

toxic than in harder water. This lack of activity is attributed to a decrease in 

the pH of the test solution which thereby decreases the concentration of the 

active, un-ionized form of the molecule.

INTRODUCTION

Quinaldine sulfate (QdSO4 ) is a candidate fish 

anesthetic (Alien and Sills, 1973). An early step 

in its development and possible registration as a 

fishery tool is definition of its toxicity to selected 

fishes in standard bioassays in waters with different hardnesses, pH's, and temperatures (Lennon,>1967). Observations also were made on the 

influence of quinaldine sulfate on bioassay media 

and on degradation of the compound.

METHODS AND MATERIALS

Static bioassays of QdSO 4 were conducted with 

3- to 14-cm fish in 15-liter glass jars according 

to the methods of Lennon and Walker (1964).

Larger fish were exposed to the anesthetic in 

45-liter polyethylene tanks. The fish were obtained from fish hatcheries, maintained under a 

fish culturist's care (Hunn, Schoettger, and 

Whealdon, 1968), acclimated according to 

standard bioassay procedures, and incinerated 

after death. Ten fish were exposed to each concentration of the anesthetic, and mortalities 

were recorded periodically during the first day 

and daily thereafter during the 96-hour tests.

Variations in test water were produced by 

adding different amounts of reconstituting salts 

to deionized water (table 1). ThepH in various 

tests was ad justed and maintained with chemical 

buffers (table 2). Temperatures of 7°, 12°, and 

17° C. were controlled by water baths.

TABIE 1. Quantities of salts and characteristics of reconstituted waters

Water 

type

very soft

soft1

hard

very hard

NaHC03

12

48

192

384

Salts added (ng/l) 

CaSO^. 2H20 MgSO,; KC1 range

Total

Hardness 2

7.5 7.5 0.5 6.4-6.8 10-13

30 30 2.0 7.2-7.6 40-48

120 120 8.0 7.6-8.0 160-180

240 240 16 8.0-8.4 280-320

Alkalinity*

10-13

30-35

110-120

225-245

1 Standard reconstituted water used in routine bioassays.

2 As mg/1 CaC03.
4 Investigations in Fish Control 48 : Bureau of Sport Fisheries and Wildlife

TABLE 2. Buffer chemicals for adjusting the pH of 

standard reconstituted water at 12° C. TABLE 3. The influence of quinaldine sulfate on the pi 

of hard and soft water test solutions

PH

Ml of solutions for 15 liters of water

IN NaOH 1M KH2P04 0.5M H3B03

6.0

6.5

7.0

7.5

8.0

8.5

9.0

9.5

10.0

-- 1.3

10.0 ,

19.0

19.0

12"'. 0

8.8

11.0

16.0

80.0

30.0

30.0

20.0

-11.5

~

__

 A

30.0

20.0

18.0

The anesthetic was dissolved in water, and 

aliquots were added to the bioassays to obtain the 

desired concentrations.

The mortality data were analyzed according to 

the method of Litchfield and Wilcoxon (1949) to 

determine LCSO's, variations, slope functions, 

and 95-percent confidence intervals.

RESULTS

Effects of QdSO4 on test solutions

Stock solutions of QdSO4 are acidic and influence thepH of bioassay water, especially softer 

waters. Stock solutions containing 75 grams of 

QdSC>4 in a liter of deionized water have a pH of 

1.5. Since different amounts of QdSO 4 are added 

to bioassays to obtain data on the survival and 

mortality of fish, the chemical properties of the 

test solutions must be considered. Concentrations ranging from 0 to 80 mg/1 ofQdSO4 were 

prepared in waters of various hardnesses, and 

the pH's were recorded (table 3). The pH in very 

soft water drops from 6.55 to 3.86 with the addition of 80 mg/1 ofQdSO4 .In harder waters which 

have a higher buffer capacity, the pH is more 

stable and decreases only one pH unit. These 

factors must be considered when assessing the 

toxicity of QdSO4 to fish.

Quinaldine 

sulfate (mgA)

0

5

20

40

60

80

pH of different test

Very soft

6.55

6.29

5.65

5.40

4.02

3.86

Soft

7.10

6.92

6.61

6.22

6.04

5.67

solutions

Hard

7.

7.

7.

7.

6.

6.

78

57

30

00

87

61

Very ha]

8.00

7.82

7.55

7.39

7.19

7.01

Species and sizes of fish

Among the coldwater species, lake trout are 

the most sensitive to QdSO4 at aU exposure 

periods (LC50 = 26.3 mg/1 at 3 hours and 15.! 

mg/1 at 96 hours) (table 4). Brook trout are 

the most resistant in 3-hour exposures 

(LC50 =83.0 mg/1), while coho salmon are 

the most resistant at 96 hours (LC50 =32.8 

and 42.0 mg/1).

Among the warmwater species, largemouth 

bass are the most sensitive to QdSO4 (96-hour 

LC50 = 6.80 mg/1). The most highly resistant 

species, carp and black bullhead, have 96-hou 

LCSO's of 72.5 and 72.0 mg/1, respectively 

(table 4). In 96-hour exposures, largemouth b 

and walleye are more sensitive than lake trout, 

and green sunfish are more sensitive than rail 

bow trout or brown trout.

Effects of temperature and water hardness

Rainbow trout are more susceptible to the 

toxic properties of QdSO4 in cold water than ii 

warm water in exposures of 1 to 6 hours (table 

This trend reverses in 96-hour exposures, ho 

ever, and the anesthetic is more toxic at 17 ° C. 

than at 7° or 12° C. At 24 hours the LC50 is 

23.8 mg/1 for 7° and 17° C., but at 12° C. the 

trout are more resistant (LC50 - 37.0 mg/1). 

Warmer temperatures cause greater variation 

in toxicity. At 17° C. the LC50 decreases fron 

47.0at 1 hour to 12.8 mg/1 at 96 hours, while 

at 7° C.theLCSO decreases from 28.9 at 1 ho 

to 23.8 mg/1 at 96 hours. The most significant
Marking and Dawson: Toxicity of Quinaldine Sulfate to Fish

TABLE 4. Toxicity of quinaldine sulfate

Species

Coho salmon 

( Oncorhynchus kisutch)

n

Rainbow trout 

(Salmo gairdneri)

Brown trout 

(Salmo trutta)

Brook trout 

( Salve linus fontinalis)

n

Lake trout 

(Salve linus namaycush)

Carp 

(Cyprinus carpio)

Black bullhead 

( Ictalurus me las)

Channel catfish 

(Ictalurus punctatus)

Green sunfish 

(Lepomis cyanellus)

Bluegill 

(Lepomis macrochirus)

Largemouth bass 

(Micropterus salmoides)

Walleye 

(Stizostedion vitreum)

Average 

length 

(cm)

4.1

11.*

4.1

3.8

4.8

13.7

4.1

4.6

4.6

5.6

4.3

4.3

4.6

5.3

Average 

weight 

(grams)

0.7

17.0

0.6

0.6

1.2

31.0

0.5

1.4

1.2

1.5

1.5

1.5

1.4

1.3

to fish in standard reconstituted water at 12° C.

LC50 and 95-percent confidence interval (mg/l) at

3 hours

80.0 

55.1-116

41.1 

38.0-44.5

55.0 

47.0-64.4

83.0 

55.5-124

39.0 

36.2-42.1

26.3 

23.1-30.0

85.4 

73.2-99.7

 

60.0 

53.7-67.1

44.1 

39.4-49.4

20.8 

18.3-23.5

17.9 

15.9-20.1

6 hours

80.0 

55.1-116

70.0 

52.1-94.0

40.0 

36.1-44.3

 

59.0 

46.6-74.7

36.0 

30.8-42.1

23.4 

20.8-26.3

80.0 

64.9-98.6

 

49.4 

43.3-56.4

 

42.3 

37.4-47.2

19.4 

17.1-22.0

17.9 

15.9-20.1

24 hours

47.5 

41.9-53.9

45.0 

42.1-48.1

37.0 

32.5-42.2

32.7 

28.5-37.5

27.2 

23.7-31.3

20.0 

16.3-24.5

16.3 

14.3-18.6

74.6 

59.3-93.8

102 

66.7-156

39.1 

34.0-45.0

23.5 

21.8-25.4

36.8 

32.5-44.7

16.0 

9.64-26.7

17.2 

15.4-19.2

% hours

32.8 

30.0-35.9

42.0 

37.6-46.9

31.8 

28.7-35.2

28.3 

25.7-31.2

22.2 

19.5-25.2

20.0 

16.3-24.5

15.5 

13.7-17.5

72.5 

59.7-88.1

72.0 

57.6-90.0

32.9 

27.4-39.5

23.5 

21.8-25.4

32.0 

27.3-37.5

6.80 

3.71-13.6

15.0 

12.1-18.5

increase in toxicity is at 17° C. in 24 and 96 

hours.

Rainbow trout are least susceptible to the toxic 

effects of QdSO4 in very soft water (12 mg/l of 

total hardness) (table 5). Extremely high concentrations of the anesthetic are necessary in 

very soft water to kill the trout in 1- to 6-hour 

exposures. None of the trout died when exposed 

for 1 hour to 140 mg/l of the drug. The decreased activity of QdSC>4 in very soft water can 

be attributed to a decrease in pH as indicated in 

tableS. At 140 mg/l ofQdSO4 , thepHof the test 

solution dropped to 3.35, which is below the pKa 

value of 5.42 (Knight et al., 1955; Sober, 1968). 

The equilibrium, therefore, is shifted in favor of 

the ionized form which is relatively unavailable 

to the fish (Sills and Alien, 1971). The extreme 

pH condition perhaps contributed to the mortality 

by stressing the fish.

In soft water (44 mg/l of total hardness), 

QdSO4 is considerably more toxic than in very 

soft water, and LCSO's range from 46.1 mg/l at 

1 hour to 31.8 mg/l at 96 hours (table 5). In 

hard water (170 mg/l of total hardness) and in 

very hard water (300 mg/l of total hardness), 

the toxicity of QdSO4 to rainbow trout is insignificantly different at each exposure (table 5). 

Also, the LCSO's change very little in 1- to 96- 

hour exposures at each water hardness, but the 

values clearly show that QdSO4 is consistently 

more toxic to trout in harder than in softer water 

at 12° C.

Effects of buffered and aged solutions of QdSO4

Selected pH's ranging from 6 to 10 were produced in soft water (44 mg/l of total hardness) 

with the buffering agents listed in table 2. These

518-291 0-73-3
6 Investigations in Fish Control 48; Bureau of Sport Fisheries and Wildlife

TABLE 5.~Tbxicity of quinaldine sulfate to rainbow trout at different tenperatures and water hardness

Water Temp, 

hardness (°C. )

soft1 7

soft1 12

soft1 17

very soft 12

hard 12

very hard 12

LC50 and 95-percent confidence interval (in ng/l) at

1 hour 3 hours

28.9 28.5 

24.3-34.4 24.7-32.1

46.1 41.1 

41.4-51.4 38.0-44.5

47.0 46.0 

39.5-55.9 40.6-52.1

133 

116-153

30.0 29.6 

27.3-32.9 28.3-31.0

28.9 28.2 

26.0-32.1 24.8-32.0

6 hours

25.8 

22.6-29.4

40.0 

36.1-44.3

42.5 

35.0-51.7

90.5 

83.2-98.4

29.6 

28.3-31.0

28.2 

24.8-32.0

24 hours

23.8 

20.3-27.9

37.0 

32.5-42.2

23.8 

19.2-29.5

65.5 

62.2-69.0

23.5 

21.3-25.9

25.0 

21.9-28.5

96 hours

23.8 

20.3-27.9

31.8 

28.7-35.2

12.8 

11.1-14.9

50.5 

46.0-55.5

22.9 

21.9-24.9

23.0 

20.1-26.3

1 Standard reconstituted water used in routine bioassays.

data were analyzed at 24 hours because QdSC>4 

does not kill the trout in shorter exposures in the 

acid waters tested, and buffer chemicals complicate the toxicity of chemicals to rainbow trout at 

very high and very low pH levels in longer exposures (Marking, 1969). Despite the buffering 

capacity of these solutions, the pH decreased proportionately with concentrations, and the changes 

were greatest atpH 6. For instance, 20.0 mg/1 

of QdSO 4 in water buffered to pH 6 decreased the

pH to 5.85, whereas 400 mg/1 of the anesthetic 

in that water decreased the pH to 3.30.

The400-mg/l concentration did not kill any 

rainbow trout at 6 hours, but they all died within 

24 hours. Again, we suspect that the fish were 

stressed by the low pH. TheQdSC>4 is more 

toxic in near neutral or basic water than in acid 

water (table 6), and LCSO's range from 20.7 to 

62.0 mg/1 at pH 10 and 6, respectively. The most

TABLE 6. Toxicity of quinaldine sulfate to rainbow trout in pH buffered water, in pH 

readjusted buffered water, and in aged (l week) pH readjusted buffered water at 12 C.

PH 

(original)

6.0

2 7.4

8.0

9.0

10.0

24-hour LC50 and

pH buffered 

tests (fresh)

62.0

54.1-71.1

37.0

32.5-42.2

23.2

20.0-27.0

25.0

22.7-27.5

20.7

18.5-23.2

95-percent confidence interval in mg/1

pH readjusted 

tests 1 (fresh)

47.1

40.7-54.5

26.3

23.5-29.4

24.4

21.0-28.3

25.7

22.4-29.4

21.1

18.0-24.8

in

pH readjusted 

tests 1 (aged)

40.0

33.0-48.6

28.2

25.6-31.1

23.8

20.6-27.6

23.8

21.6-26.2

15.9

13.5-18.8

1 Readjusted to desired pH at all concentrations of quinaldine sulfate.

2 Standard reconstituted water.
Marking and Dawson: Toxicity of Quinaldine Sulfate to Fish

significant decrease in activity is from pH 7.4 

to pH 6.

In tests in alkaline waters of pH 8, 9, and 10, 

where the pH was readjusted to original buffered 

pH's at all concentrations of QdSC>4 , the toxicity 

was insignificantly different than unadjusted 

tests (table 6). The toxicity of QdSO4 increased 

in near neutral and acid waters when the pH was 

read justed to 7.4 and 6.0, and LCSO's are 26.3 

and 47.1 mg/1, respectively. Again, QdSO4 is 

more toxic in high pH waters.

Concurrent with the fresh, pH readjusted tests, 

similar concentrations of QdSO4 were pH readjusted and aged for 1 week prior to introducing 

rainbow trout into the bioassays. The aged, pH 

readjusted solutions of QdSO4 remain as active 

as fresh, pH readjusted solutions at the pH's 

tested (table 6). In fact, the aged, pH readjusted 

solutions are significantly more toxic at pH 10.

DISCUSSION

Quinaldine sulfate is consistently less toxic to 

fish than quinaldine (Marking, 1969). The 96-hour 

LCSO's forQdSO 4 when tested against brook 

trout and channel catfish were 20.0 and 32.9 

mg/1, respectively. The 96-hour LCSO's for 

quinaldine were 12.0 mg/1 for brook trout and 

19.9 mg/1 for channel catfish. However, when the 

concentrations are computed on the basis of active ingredients, the formulations are approximately equal in activity.

The activity of QdSO4 is similar at various 

temperatures to that of quinaldine (Marking, 

1969). Both compounds are more toxic at colder 

temperatures in 1- to 6-hour exposures, but the 

trend begins to change at 24 hours and reverses 

at 96 hours for the extreme temperatures. These 

data suggest that exposures at warmer temperatures are perhaps safer (less toxic), providing 

the exposures are short. In contrast, MS-222 

(a fish anesthetic) is more toxic to fish at warmer 

temperatures (Marking, 1967).

Tests in very soft and acid water indicate that 

the activity of QdSO4 is decreased considerably 

in these waters. In agreement, Schoettger and 

Julin( 1969) and Sills and Alien (1971) report that 

quinaldine loses its effectiveness in solutions

having pH values less than 6. Since rainbow trout 

are generally intolerant to high or low pH's, we 

suspect that the low pH is more responsible for 

mortality than the QdSO 4 in this water.

CONCLUSIONS

1. QdSO 4 is toxic to fish, and the 96-hour 

LCSO's for 12 species in standard reconstituted water range from 6.80 to 72.5 mg/1 

Carp are most resistant, while lake trout are 

most sensitive.

2. QdSO4 is more toxic to rainbow trout in cold 

water than in warm water in 1- to 6-hour exposures, but the trend reverses at 96 hours.

3. The anesthetic is more toxic in hard than in 

soft water, but the increased pH in hard water 

perhaps contributes to the greater toxicity.

4. Higher concentrations of QdSO4 decrease the 

pH of buffered and nonbuffered test solutions 

significantly, thereby decreasing the concentration of the un-ionized quinaldine. We suspect that the low pH stressed the fish and 

contributed to the mortality. The anesthetic 

is consistently toxic in buffered solutions of 

pH 8, 9, and 10, but the drug is considerably 

less toxic at pH 6.

5. The anesthetic in reconstituted water remains 

as toxic in solutions aged for 1 week as in 

fresh solutions.

REFERENCES

Alien, John L.e and Joe B. Sills.

1973. Preparation and properties of quinaldine sulfate, 

an improved fish anesthetic. U.S. Bureau of Sport 

Fisheries and Wildlife. Investigations in Fish Control 

No. 47.

Hunn, Joseph B., Richard A. Schoettger, and Everett W. 

Whealdon.

1968. Observations on the handling and maintenance of

bioassay fish. The Progressive Fish-Culturist,

vol. 30, no. 3, p. 164-167.

Knight, Samuel B.. R. H. Wallick, and Carolyn Bolch.

1955. The ultraviolet spectra and the dissociation constants of the monochloroquinolines and the 

monomethylquinolines. Journal of the American 

Chemical Society, vol. 17, p. 2577-2579.
8 Investigations in Fish Control 48 : Bureau of Sport Fisheries and Wildlife

Lennon, Robert E.

1967, Clearance and registration of chemical tools 

for fisheries. The Progressive Fish-Culturist, 

vol. 29, no. 4, p. 187-193.

Lennon, Robert E.t and Charles R. Walker.

1964. Laboratories and methods for screening 

fish-control chemicals. U.S. Bureau of Sport 

Fisheries and Wildlife, Investigations in Fish 

Control No. 1, Circular 185, 15 p.

Litchfield, J. T., Jr0 and F. Wilcoxon.

1949. A simplified method of evaluating doseeffect experiments. Journal of Pharmacology 

and Experimental Therapeutics, vol. 96, no. 2, 

p. 99-113.

Marking, Leif L.

1967. Toxicity of MS-222 to selected fishes. U.S. 

Bureau of Sport Fisheries and Wildlife, Investigations in Fish Control No. 12. 10 p.

Marking, Leif L.

1969. Toxicity of quinaldine to selected fishes. 

U.S. Bureau of Sport Fisheries and Wildlife, Investigations in Fish Control No. 23. 10 p.

Schoettger, Richard A., and Arnold M. Julin.

1969. The efficacy of quinaldine as an anesthetic 

for seven species of fish. U.S. Bureau of 

Sport Fisheries and Wildlife, Investigations in 

Fish Control No. 22. 10 p.

Sills, Joe B., and John L. Alien.

1971. The influence of pH on the efficacy and residues 

of quinaldine. Transactions of the American Fisheries Society, vol. 100, no. 3, p. 544-545.

Sober, Herbert A.

1968. Handbook of biochemistry. Selected data for 

molecular biology. The Chemical Rubber Company, 

Cleveland, Ohio, p. J-182.

Alien, John L.t and Joe B. Sills.

Preparation and properties of quinaldine sulfate, an 

improved fish anesthetic. U.S. Bureau of Sport Fisheries and Wildlife, Investigations in Fish Control 

No. 47.

Gilderhus, Philip A.t Bernard L. Berger, Joe B. Sills, and

Paul D. Harmon.

The efficacy of quinaldine sulfate (QdSC>4 ) as an 

anesthetic for freshwater fish. U.S. Bureau of Sport 

Fisheries and Wildlife, Investigations in Fish Control 

No. 49.

Luhnlng, Charles W., and Paul D. Harman.

1971. Sampling of fish muscle for MS-222 and quinaldini 

residues. Journal of the Fisheries Research Board of 

Canada, vol. 28, no. 1, p. 113-115.

Sills, Joe B., and Paul D. Harman.

1970. Efficacy and residues of quinaldine sulf ate, an 

anesthetic for striped bass (Roccus saxatilis). Proceedings of 24th Annual Conference of the Southeastern Association of Game and Fish Commissioners, 

vol. 24, p. 546-549.

Walker, Charles R^ and Richard A. Schoettger.

1967. Residues of MS-222 in four salmonids following 

anesthesia. U.S. Bureau of Sport Fisheries and Wildlife, Investigations in Fish Control no. 15, lip.
INVESTIGATIONS IN FISH CONTROL

49. The Efficacy of Quinaldine Sulf ate as an 

Anesthetic for Freshwater Fish

By Philip A. Gilderhus, Bernard L. Berger, 

Joe B. Sills, and Paul D. Harman

United States Department of the Interior, Rogers C. B. Morton, Secretary

Nathaniel P. Reed, Assistant Secretary for

Fish and Wildlife and Parks,

Fish and Wildlife Service

Bureau of Sport Fisheries and Wildlife, Spencer H. Smith, Director

Washington, D.C. April 1973
CONTENTS

Page

Abstract. ...................................... 3

Introduction .................................... 3

Methods and Materials ............................. 3

Results ....................................... 5

Reactions of fish .............................. 5

Efficacy of the anesthetic ........................ 5

Discussion ..................................... 8

Conclusions .................................... 8

References ..................................... 8
THE EFFICACY OF QUINALDINE SULFATE 

AS AN ANESTHETIC FOR FRESHWATER FISH

By Philip A. Gilderhus, Bernard L. Berger, Joe B. Sills, 

and Paul D. Harman

ABSTRACT. Quinaldine sulfate (QdSO^), an improved formulation of 

the fish anesthetic quinaldine, was tested for its efficacy on 15 species of 

freshwater fish. The new crystalline formulation is water soluble and thus 

easier to use than is practical grade quinaldine. QdSO^ anesthetizes most 

salmonids at 25 mg/1 in less than 4 minutes and the fish recover in 1 to 

13 minutes in fresh water. The effective concentrations for several warmwater species varied from 15 mg/1 for bluegills to 60 mg/1 for channel 

catfish. Fish were held for up to 60 minutes in effective concentrations 

without suffering mortalities. The efficacy of the anesthetic was little affected by water temperature, but the compound lowers the pH of some soft 

waters to below 6, the point at which it becomes ineffective as an anesthetic. All fish retained some reflex action and thus, some large fish were 

difficult to handle.

INTRODUCTION

Quinaldine (2-methylquinoline) has been 

used to anesthetize fish for spawning, marking, 

measuring, and long-distance transport of 

fish. Schoettger and Julin (1969) demonstrated 

that practical grade quinaldine anesthetizes 

several species of coldwater and warmwater 

fish to a handleable condition at 15 to 70 

mg/1 in 2 minutes or less. Fish were held for 

up to 6 hours in effective concentrations and 

recovered in less than 1 hour after their return to fresh water.

Practical grade quinaldine (liquid, 95 percent), 

however, is insoluble in water and has a disagreeable odor. To overcome these disadvantages, Alien and Sills (1973) synthesized 

quinaldine sulfate (QdSO^), a crystalline salt 

of quinaldine, which is water soluble and has 

little or no odor. Marking and Dawson (1973) 

have investigated the toxicity of quinaldine 

sulfate and found the material generally of 

comparable or lower toxicity than practical 

grade quinaldine (Marking, 1969) on an active

ingredient basis using fish of comparable size 

at the same water temperature.

The efficacy of QdSC^. was tested on freshwater fish to provide guidelines for use by 

fishery workers and to provide the proof of 

efficacy required by the regulatory agencies 

for registration.

METHODS AND MATERIALS

The quinaldine sulfate (59.3 percent quinaldine) used in these tests was formulated at the 

Southeastern Fish Control Laboratory at 

Warm Springs, Georgia. This compound is an 

experimental drug and is not registered for 

use as an anesthetic for fish. Aliquots of 

anesthetic were weighed individually for each 

concentration or test vessel.

Depending on the availability of fish, the 

anesthetic was tested on some species at the 

Fish Control Laboratory, La Crosse, Wisconsin, on some at the Warm Springs laboratory, and on some at both laboratories. Field
Investigations in Fish Control 49: Bureau of Sport Fisheries and Wildlife

tests were conducted at several fish hatcheries where fish were anesthetized during 

spawning operations.

Tests using fingerling-size fish were conducted in 15-liter glass jars. Larger fish 

were exposed to the anesthetic in the laboratory and field in 45- and 100-liter polyethylene tanks. Water temperatures were adjusted 

and maintained by placing the test vessel in a 

water bath of the appropriate temperature.

The species of fish exposed to the anesthetic were coho salmon (Oncorhynchus 

kisutch), rainbow trout (Salmo qairdneri), 

brown trout (Salmo trutta), brook trout 

(Salvelinus fontinalis), lake trout (Salvelinus 

namaycush), northern pike (Esox lucius), 

goldfish (Carassius auratus), carp (Cyprinus 

carpio), white amur (Ctenopharyngodon idella), 

white sucker (Catostomus commersoni), black 

bullhead (Ictalurus melas), channel catfish 

(Ictalurus punctatus), bluegill (Lepomis 

macrochirus), largemouth bass (Micropterus 

salmoides), and walleye (Stizostedion vitreum).

The fish for laboratory tests were obtained 

from Federal and State fish hatcheries or, in

the case of small coho salmon and rainbow 

trout, hatched and reared at the La Crosse 

laboratory. All fish tested in the laboratories 

were maintained as described by Hunn et al. 

(1968). The fish were acclimated to the test 

water and temperature for 16 to 24 hours before their exposure to the anesthetic.

The laboratory tests at La Crosse were conducted in well water and soft, reconstituted 

water. Those at Warm Springs were conducted 

in limed spring water (table 1). The field tests 

were conducted in the water supplies of the 

respective fish hatcheries (table 2).

TABLE 1. Characteristics of waters used in laboratory 

tests of quinaldine sulfate as an anesthetic for fish

Source Type pH

Total 

hardness

Total 

alkalinity

Well La Crosse

Reconstituted La 

Crosse

Spring Warm Springs

hard 7.6-7.9 238-258 218-236

soft 7.2-7.6 40-48 30-35

soft 6.8-7.0 20

TABLE 2. Characteristics of hatchery water supplies used in tests of QdSO^ to

anesthetize adult fish

Location

Platte River SFH1 

Michigan

Manchester NFH2

Iowa

Manchester NFH 

Iowa

Osceola SFH 

Wisconsin

Crystal Springs SFH 

Minnesota

Lansing SFH 

Iowa

Lansing SFH 

Iowa

Species 

tested

coho salmon

rainbow trout

brown trout

brook trout

lake trout

northern pike

walleye

Water 

temp. 

(°C.)

6

9

8

9

8

5

10

PH

7.8

7.5

 

8.1

7.5

9.2

9.2

Total 

alkalinity 

(n /D

150

172

 

171

257

141

133

Total 

hardness 

(n /D

168

215

 

208

280

144

164

1 State fish hatchery.

2 National fish hatchery.
Gilderhus, Berger, Sills, and Harman: Efficacy of Quinaldine Sulfate as an Anesthetic

The temperatures of test solutions were 

7° 12°, 17°, 22°, and 27° C. at La Crosse and 

19 C. at Warm Springs. Field tests were conducted at the existing temperatures of the 

hatchery water supplies.

Schoettger and Julin (1967) defined loss of 

equilibrium, Stage 2, as the stage of anesthesia at which locomotion ceases, opercular 

rate slows, but reflex response to pressure on 

the caudal fin or peduncle is retained. In their 

tests with quinaldine, Schoettger and Julin 

(1969) found that the depth of anesthesia in 

fish rarely progresses beyond loss of equilibrium, Stage 2. Therefore, the majority of our 

tests were designed to define the most economical concentrations which would anesthetize 100 percent of the individual fish exposed, to loss of equilibrium, Stage 2, in 4 

minutes or less. These criteria appear to 

satisfy the requirements for most of the field 

uses of fish anesthetics.

RESULTS

Reactions of fish

The reactions of fish to quinaldine sulfate 

were similar to their reactions to practical 

grade quinaldine as described by Schoettger

and Julin (1969). Initially the fish show a short 

period of increased activity, but the anesthetization progresses rapidly to loss of equilibrium, Stage 2, and rarely progresses beyond that stage.

The fish usually retained reflex action which 

could be triggered by tactile stimuli. The reflex action in large adult fish sometimes made 

them difficult to handle without injury to the 

fish. Northern pike were most likely to display this action and salmonids the least.

Efficacy of the anesthetic

Twenty to 30 mg/1 of QdSO-t anesthetized 

the five species of salmonids to loss of equilibrium, Stage 2, in approximately 4 minutes 

or less (table 3). Twenty-five mg/1 of QdSO^ 

(15 mg/1 of quinaldine) were effective on most 

species and sizes of salmonids, comparing 

favorably with the 15 to 16 mg/1 of quinaldine 

found to be effective by Schoettger and Julin 

(1969). All of the salmonids in our tests recovered in fresh water within 1 to 13 minutes 

compared to 3 to 21 minutes for salmonids in 

similar exposures to quinaldine as stated by 

Schoettger and Julin (1969). Fish were retained up to 60 minutes in loss of equilibrium, 

Stage 2, without any apparent harm.

TABLE 3. Efficacy of quinaldine sulfate as an anesthetic for salmonids in laboratory tests

Mean Type 

Species weight of jro 

(grams) water

Concen- Number Exposure 

, v tration of time 

(mg/1) fish (min. )

Coho salmon 12 hard 12 20 15 15-60

Rainbow trout 450 hard 7 25 15 15

Do. 80 hard 12 25 15 15-60

Do. 25 hard 17 25 30 15-60

Brown trout 18 hard 7 25 15 15-60

Do. 16 hard 12 25 15 15-60

Do. 16 hard 17 25 15 15-60

Brook trout 27 hard 7 25 15 15-60

Do. 27 hard 12 25 15 15-60

Do. i.l soft 12 25 5 15

Lake trout 25 hard 7 25 10 15-30

Do. 30 hard 12 25 15 15-60

Do. 25 hard 17 25 10 15-30

Time in minutes to

Loss of 

equilibrium Recovery 

Stage 2

0.9-1.3 1.0-2.8

1.0-1.8 6.0-8.5

1.0-2.0 2.5-5.7

0.6-1.0 1.0-4.2

0.7-1.0 5.0-10.0

0.9-1.2 3.5-8.5

0.5-0.9 3.4-6.0

1.0-1.6 3.0-8.0

2.0-3.0 2.3-6.0

1.1-1.2 2.2-3.0

0.9-1.2 8.0-13.0

0.8-1.5 3.5-8.0

0.7-1.2 2.2-5.1
6 Investigations in Fish Control 49: Bureau of Sport Fisheries and Wildlife

The same concentrations of QdSCU which 

were effective in the laboratory (20 to 25 

mg/1) were effective on larger trout and salmon in field tests (table 4). The large fish exhibited stronger reflex actions when touched 

or gently squeezed.

The warmwater species generally required 

higher concentrations of the anesthetic than 

did the salmonids. Northern pike, black bullheads, and channel catfish were the most resistant fishes requiring up to 65 mg/1 of 

QdSO^. for rapid anesthetization (table 5). 

Bluegills were the most susceptible, being 

anesthetized by 15 to 25 mg/1. On an active 

ingredient basis our 9 to 15 mg/1 for bluegills and 15 mg/1 for largemouth bass compare very favorably with the 15 mg/1 found to 

be effective on both species by Schoettger and 

Julin (1969). The warmwater fish recovered 

after 1 to 22 minutes in fresh water.

The speed at which a given concentration of 

QdSO4 induced anesthesia was somewhat related to the size of fish, with larger fish requiring slightly longer times to reach the 

same stage (table 6). The differences were 

minimal and would not usually justify the 

use of higher concentrations on larger fish. 

When the size of fish was constant, higher 

concentrations sometimes induced anesthesia 

more rapidly. However, reducing the time 

needed for anesthetization by 1 to 2 minutes 

does not generally warrant the use of greatly 

increased concentrations.

The water temperature, in most cases, did 

not appreciably affect the efficacy of the 

anesthetic. Among salmonids, a single concentration was usually effective on any particular species at all temperatures. Northern 

pike and black bullheads were anesthetized by 

somewhat lower concentrations at temperatures of 22° to 27° C. than at 12° C.

TABLE 4. Efficacy of quinaldine sulfate as an anesthetic for adult fish at field

installations

Species 

and 

location

.No. 

of 

fish

Average 

weight 

of fish 

(kg)

Effective 

concentration

(ne/D

Time in minutes to

Loss of 

equilibrium 

Stage 2

Recovery in 

fresh water

Coho salmon 

Platte River SFH1, Michigan

Rainbow trout 

Manchester NFH2 , Iowa

Brown trout 

Manchester NFH, Iowa

Brook trout 

Osceola SFH, Wisconsin

Lake trout 

Crystal Springs SFH, Minnesota

Northern pike 

Lansing SFH, Iowa

Walleye 

Lansing SFH, Iowa

3

12

21

31

6

9

3

3.5

0.3

1.1

0.7

1.5

1.6

0.8

25

25

25

25

25

30

20

3.3

0.9-1.5

0.8-1.2

0.9-2.3

2.5-3.0

6.0-11.5

2.1-3.2

3.5

3.0-4.0

5.3-8.3

2.0-4.5

 

9.8-22.0

3.0-18.8

1 State fish hatchery.

2 National fish hatchery.
Gilderhus, Berger, Sills, and Harman: Efficacy of Quinaldine Sulfate as an Anesthetic 7

TABLE 5. Efficacy of qulnaldine sulfate as an anesthetic for warmwater fishes in laboratory tests

Species

Mean 

weight 

(grams)

Type 

of 

water

Temp. 

(°C.)

Concentration 

(mg/1)

Number 

of 

fish

Exposure 

time 

(min.)

Time in minutes to

Loss of 

equilibrium 

Stage 2

Recovery

Northern pike 115

Do. 115

Do. 115

Do. 115

Carp 60

Do. 387

Do. 387

White amur 227

Black bullhead 208

Do. 129

Do. 129

Channel 

catfish 1.8

Do. 1.5

Do. 1316

Bluegill 77

Do. 80

Do. 142

Largemouth 

bass 12

Do. 908

soft

hard

soft

soft

hard

hard

hard

soft1

hard

hard

hard

hard

hard

soft1

hard

hard

soft1

hard

soft1

7 40

12 40

17 40

22 25

12 35

22 25

27 25

19 30

12 50

22 25

27 ' 25

12 60

17 60

19 65

17 15

27 25

19 20

17 25

19 30

5 15 3.3-4.3

5 15 2.5-4.2

5 15 1.3-2.6

5 15 2.5-2.9

15 15-60 2.3-2.9

10 5.5-15 1.7-4.5

5 15 3.6-3.8

3 30 1.1-1.6

10 5.5-15 2.5-3.6

10 5.5-15 2.8-3.7

5 15 3.7

10 5.5-15 1.3-3.6

5 15 0.9-1.1

20 30 2.0-3.0

5 15 1.7-2.1

10 5.5-15 0.7-1.2

43 30 2.0-3.0

5 15 1.1-1.5

30 30 1.8-3.0

10.0-11.7

4.0-6.1

2.0-3.0

0.9-1.1

6.3-15.9

2.5-5.0

1.5-6.2

4.0-6.0

4.0-22.0

1.7-4.3

2.0-3.0

3.0-5.5

1.8-6.2

3.0-8.0

2.0-3.7

2.0-2.5

1.0-3.0

2.8-3.5

3.0-10.0

1 Spring water - Warm Springs Laboratory.

TABLE 6. Examples of differences in rate of anesthesia among different size 

to quinaldine sulfate in well water

Species

Rainbow trout

Do.

Do.

Do.

Lake trout

Do.

Mean 

weight 

(grams)

450

1.5

450

25

25

1.5

Temp.

(°c.)

12

12

17

17

17

17

Concentration 

(mg/1)

25

25

25

25

25

25

fish exposed

Time to loss of 

equilibrium, Stage 2 

(min. )

0.8-1.

0.5

0.8-1.

0.6-0.

0.7-1.

0.5-0.

5

3

9

2

6
8 Investigations in Fish Control 49: Bureau of Sport Fisheries and Wildlife

The hardness and pH of the water have a 

pronounced effect on the efficacy of QdSO^. 

In soft, poorly-buffered water, the addition of 

60 mg/1 of QdSO4 reduces the pH to 6.04 

(Marking and Dawson, 1973). At that pH, a 

significant portion of the quinaldine ionizes 

and becomes unavailable to the fish (Schoettger and Julin, 1969; Sills and Alien, 1971). 

The relationship of hardness and pH to efficacy was demonstrated by comparing the efficacy on northern pike in two different waters 

at 12° C. Forty mg/1 were effective in hard 

water and 60 mg/1 were ineffective in soft 

water.

DISCUSSION

Quinaldine sulfate proved to be an effective 

anesthetic for all of the species of fish on 

which it was tested. The fish were anesthetized to loss of equilibrium, Stage 2, in about 

4 minutes or less, and all species but channel 

catfish survived 60 minutes of exposure to 

effective concentrations. A rather narrow 

range of concentrations (20 to 35 mg/1) was 

effective on salmonids, cyprinids, and centrarchids. Higher concentrations (40 to 65 

mg/1) were required for northern pike and the 

ictalurids. The anesthetic is effective over a 

wide range of temperatures (7° to 27° C.) and 

in soft and hard waters. The species of fish 

used in the tests of QdSQ/. represent a wide 

range of physiological characteristics. Thus, 

the concentrations of 20 to 65 mg/1 and exposures of up to 1 hour should serve as guidelines for use on most species of fish.

The only limiting factor on the efficacy of 

QdSO^ is a pH below 6, at which the compound 

ionizes and becomes ineffective. The anesthetic itself is acidic and concentrations of 20 

mg/1 in very soft water (total hardness of 10 

to 13 mg/1) and 60 mg/1 in soft water (total 

hardness of 40 to 48 mg/1) lower the pH to 

near or below that point (Marking and Dawson, 

1973). If the pH of the anesthetic solution is 

excessively low, it should be buffered back to 

the range of 6.5 to 7.0 with NaHCO3 .

Schoettger and Julin (1969) stated that 1 

ml of quinaldine would anesthetize 94.5 kg of 

rainbow trout before the time to anesthetization increased. The effective concentrations 

of QdSO^ were comparable, on an active ingredient basis, to those of practical grade 

quinaldine given by Schoettger and Julin 

(1969). By inference then, the weight of fish 

which can be anesthetized per unit of active 

ingredient of quinaldine and QdSO^ are likely 

to be similar.

The major assets of QdSO,/., like those of 

quinaldine, are rapid anesthetization and a 

long safe-exposure time. In addition, QdSO^. 

is more convenient to use than quinaldine because it does not have to be put into solution 

with an organic solvent. As with quinaldine, 

QdSO,; does not completely inhibit reflex response. The reflex movements of large fish 

may be objectionable to some workers. A 

given degree of reflex response, however, 

may be a hindrance to one person and of no 

consequence to another.

CONCLUSIONS

1. Quinaldine sulfate is an effective anesthetic 

for most species of freshwater fish in concentrations of 20 to 65 mg/1.

2. The crystalline, water soluble material is 

convenient to handle and is as effective as 

practical grade quinaldine, on an active 

ingredient basis.

3. The efficacy of QdSCX; is not greatly influenced by water temperature or size of 

fish.

4. In soft waters, high concentrations of 

QdSO^ lower the pH of the solution, 

rendering the anesthetic ineffective.

5. The reflex action retained by fish under 

anesthesia may interfere with the handling 

of large fish.

REFERENCES

Alien, John L., and Joe B. Sills. 

1973. Preparation and properties of quinaldine 

sulfate, an improved fish anesthetic. U.S. Bureau 

of Sport Fisheries and Wildlife, Investigations in 

. Fish Control No. 47.
Gilderhus, Berger, Sills, and Harman: Efficacy of Quinaldine Sulfate as an Anesthetic 9

Hunn, Joseph B., Richard A. Schoettger and Everett W. 

Whealdon.

1968. Observations on handling and maintenance of 

bioassay fish. The Progressive Fish-Culturist, 

vol. 30, No. 3. p. 164-167.

Marking, Leif L.

1969. Toxicity of quinaldine to selected fishes. 

U.S. Bureau of Sport Fisheries and Wildlife, Investigations in Fish Control No. 13. 10 p.

Marking, Leif L.t and Verdel K. Dawson.

1973. Toxicity of quinaldine sulfate (QdSO^ ) 

to fish. U.S. Bureau of Sport Fisheries 

and Wildlife. Investigations in Fish Control 

No. 48.

Schoettger, Richard A., and Arnold M. Julin.

1967. Efficacy of MS-222 as an anesthetic on four 

salmonids. U.S. Bureau of Sport Fisheries and 

Wildlife, Investigations in Fish Control No. 13. 

15 p.

Schoettger, Richard AM and Arnold M. Julin.

1969. Efficacy of quinaldine as an anesthetic for 

seven species of fish. U.S. Bureau of Sport Fisheries and Wildlife, Investigations in Fish Control No. 22. 8 p.

Sills, Joe B.» and John L. Alien.

1971. Relation of pH to efficacy and residues of 

quinaldine. Transactions of the American Fisheries Society, vol. 100, No. 3, p. 544-545.
INVESTIGATIONS IN FISH CONTROL

SO. Residue of Quinaldine in Ten Species of Fish 

Following Anesthesia with Quinaldine Sulfate

By Joe B. Sills, John L. Alien, .Paul D. Harman, 

and Charles W. Luhning

United States Department of the Interior, Rogers C. B. Morton, Secretary

Nathaniel P. Reed, Assistant Secretary for 

Fish and Wildlife and Parks 

Fish and Wildlife Service

Bureau of Sport Fisheries and Wildlife, Spencer H. Smith, Director

Washington, D.C. April 1973
CONTENTS

Page

Abstract. ...................................... 3

Introduction. .................................... 3

Methods and materials ............................. 3

Results. ....................................... 4

Discussion ..................................... 7

Conclusions. .................................... 7

References ..................................... 9
RESIDUE OF QUINALDINE IN TEN SPECIES OF FISH FOLLOWING 

ANESTHESIA WITH QUINALDINE SULFATE

By Joe B. Sills, John L. Alien, Paul D. Harman,

and Charles W. Luhning

Fish Control Laboratories, La Crosse, Wisconsin 

and Warm Springs, Georgia

ABSTRACT. The concentration and persistence of residues of the 

anesthetic quinaldine in five species of both coldwater and warmwater 

fishes were measured following treatment with the new formulation 

quinaldine sulfate. Quinaldine accumulated in relation to increasing 

temperature, treatment concentration, and length of exposure. Mean 

concentrations of quinaldine residues ranged from 1.18 to 8.31 //g/g 

for the 0-hour withdrawal time. Initial residues were higher in warmwater species than in salmonids. Although a wide range of residue concentrations (0.80-9.34 #g/g) occurred immediately after exposure, these 

residues are dissipated rapidly when the fish are placed in fresh water. 

All fish tested after 24 hours of withdrawal in fresh water contained 

0.01 x/g/g or less of quinaldine residue with the exception of the rainbow 

trout treated at 7° C.

INTRODUCTION

Quinaldine sulfate was prepared by Alien 

and Sills (1973) as an improved form of the 

fish anesthetic quinaldine. In order to register this formulation, the concentration and

TABLE 1. Species of fish analyzed for quinaldine 

residues following anesthesia with quinaldine sulfate

Common Name Scientific Name

Coho salmon 

Brown trout 

Rainbow trout 

Lake trout 

Brook trout 

Northern pike 

Channel catfish 

Largemouth bass 

Bluegill 

Walleye

Oncorhynchus kisutch 

Salmo trutta 

Salmo gairdneri 

Salvelinus namaycush 

Salvelinus fontinalis 

Esox lucius 

Ictalurus punctatus 

Micropterus salmoides 

Lepomis macrochirus 

Stizostedion vitreum

persistence of residues in fish tissues must 

be known. Sills and Harman (1970) determined 

residue levels in striped bass (Morone saxatilis) following anesthesia with the quinaldine 

salt. In the present study, 10 species of coldwater and warmwater fishes (table 1) were 

anesthetized with quinaldine sulfate at various 

concentrations, temperatures, and times, and 

muscle tissue was analyzed for quinaldine 

residue.

METHODS AND MATERIALS

Ten species of fish used in this study were 

treated with efficacious concentrations of 

quinaldine sulfate by Gilderhus et al. (1973). 

Temperatures of treatment ranged from 7° to 

19° C., and exposure times ranged from 5.5 

to 30 minutes. A wide range of concentrations 

(20 to 65 mg/1) was necessary because of the 

variety of species and temperatures involved.
Investigations in Fish Control 50; Bureau of Sport Fisheries and Wildlife

Withdrawal times began when exposed fish 

were placed in fresh, flowing water for recovery. Three fish were used for residue 

analysis at 0, 1, 2, 4, either 6 or 8, and 24 

hours. Samples of muscle tissue were obtained from homogenized fillets (Luhning and 

Harman, 1971) and were analyzed for quinaldine by gas chromatography using the methods 

of Alien and Sills (1970a and 1970b). Three 

samples were analyzed at each withdrawal. 

Quinaldine residues were measured to 0.01 

I/g/g, and any value less than this was considered zero.

RESULTS

Coho salmon

posures after 24 hours of withdrawal from the 

anesthetic.

Brown trout

Brown trout were exposed to 25 mg/1 of 

quinaldine sulfate at 12° C. for both 5.5.and 

15 minutes. Quinaldine residues ranged from 

a mean of 1.44 j/g/g after 5.5 minutes of exposure to 1.67 |/g/g after 15 minutes of exposure. No detectable residue (less than 0.01 

H g/g) remained after 8 hours of withdrawal 

from the anesthetic (table 3).

TABLE 3.--Residues of quinaldine in muscle of brown 

trout after anesthesia with 25 mg/1 of quinaldine 

sulfate at 12° C.

Coho salmon were the largest fish t

(table 2). They were

quinaldine sulfate at

 L11UC.L VdJOG! colcU ^£*rl I

treated with 25 mg/1 of control

4° C. Mean quinaldine

^ 0-hour residues for the 0-hour withdrawal interval "

were 1.18 and 1.78 ft g/g for the 5. 5- andlS- ^-^^

minute exposures, respectively. Quinaldine 2-hour

residue was less than 0.01 j/g/g for both ex- ' 4-hour

8- hour

( minutes)

0

15

15

15

15

15

(grams)

582

646

525

521

584

592

Mean

O.OO2

1.67

0.65

0.09

0.02

0.00

Range

0.00

1.32-2.14

0.48-0.86

0.05-O.U

0.02-0.02

0.00

TABLE 2. Residues of quinaldine in coho salmon muscle

following anesthesia with 25 mg/1 of quinaldine sul- 24-hour 15 515 0.00 0.00

fate at 4U C.

Withdrawal

interval

control

0-hour

1-hour

2-hour

4- hour

8 -hour

24- hour

0-hour

8- hour

24-hour

Exposure

time

( minutes)

0

5.5

5.5

5.5

5.5

5.5

5.5

15

15

15

Mean

weight

(kg)

2.03

4.07

2.79

3.83

3.86

3.25

3.77

3.96

3.63

2.69

0-hour

Residues (i/g/g) 1

Quinaldine 2-hour

Mean

O.OO2

1.18

0.09

0.03

0.01

0.00

0.00

8-hour Range

5.5

5.5

5.5

542

555

492

n 1 Each mean value represents the 

u»uu

yses.

r>3 2 Values less "than 0.01 vg/g are

0.07-0.14

1.44

0.03

0.00

average of

1.21-1.81

0.02-0.04

0.00

three analreported as 0.00.

o.Qi-0.06 Rainbow trout

o.oo-o.oi Rainbow trout were tested

o.oo Fish weighing from

most extensively.

approximately 100 to 550

grams which had been exposed to 25 mg/1 of 

quinaldine sulfate were analyzed for quinaldine residue. At 12° C.. fish 1.78

0.00

0.00

1.03-2.46 , . - _

anesthetic were 5.5

exposures to the

o and 15 minutes. At 7 and

o.oo 17° c> the fish were exposed to the anesthetic

o.oo for 15 minutes (table 4). A quinaldine

\iroa Hol-onl-aHIo immorli atolv fnllnwinff

1 Each mean value represents the average of

analyses. 

2 Values less than 0.01 i/g/g are reported as

residue

pxnnsthree ure to quinaldine sulfate and the initial residue

was higher as the temperature and exposure

0.00. . . j

time increased.
Sills, Alien, Barman, and Luhning: Residue of Quinaldine in Ten Species of Fish

TABLE 4. Residues of quinaldine in muscle of rainbow 

trout anesthetized with 25 mg/1 of quinaldine sulfate 

at three temperatures

Withdrawal 

interval

Treatment

Exposures 

(minutes)

Temp.

(°c.)

Mean 

Weight 

(grams)

Residues Ug/g) 1 

Quinaldine

Mean Range

and 15 minutes contained a mean residue of 

quinaldine of 1.80 and 2.62 //g/g, respectively. 

After 24 hours of withdrawal at 12° C., the 

quinaldine residue concentrations had fallen 

below 0.01 //g/g in both the 5.5- and 15- 

minute exposures. The rainbow trout treated 

at 17° C. contained a mean residue of 4.51

control

0-hour

1-hour

2 -hour

4-hour

24-hour

control

0-hour

1-hour

2-hour

4-hour

8-hour

24-hour

0-hour

1-hour

2 -hour

4 -hour

8-hour

24-hour

control

0-hour

1-hour

2 -hour

4-hour

8-hour

1 Tnn^V. *nn

0

15

15

15

15

15

0

15

15

15

15

15

15

5.5

5.5

5.5

5.5

5.5

5.5

0

15

15

15

15

15

7

7

7

7

7

7

12

12

12

12

12

12

12

12

12

12

12

12

12

17

17

17

17

17

17

384

419

335

480

452

547

135

452

460

357

327

403

455

142

131

145

118

93

111

135

392

433

440

360

466

2 0

3

1

0

0

0

0

2

0

0

0

0

0

1

0

0

0

0

0

0

4

2

1

1

0

.00

.53

.99

.67

.64

.17

.00

.62

.73

.22

.04

.00

.00

.80

.32

.10

.03

.01

.00

.00

.51

.02

.44

.11

.44

2

1

0

0

0

0

0

0

0

1

0

0

0

0

2

1

0

0

0

J.-1-

0.00

.40-4

.20-3

.64-0

.46-0

.15-0

0.00

.80-5

.46-1

.16-0

.01-0

0.00

0.00

.10-2

.30-0

.08-0

.03-0

.01-0

0.00

0.00

.08-6

.55-2

.77-2

.90-1

.38-0

.80

.22

.72

.75

.18 

.83

.28

.26

.06

.40

.33

.11

.03

.01

.25

.87

.17

.33

.54

//g/g oi quinaioine at u-nour withdrawal ana

0.44 //g/g quinaldine after 8 hours of withdrawal. A 24-hour withdrawal was not available for this set of samples.

Lake trout and brook trout

Lake trout exposed to the anesthetic at

12 C. for 5.5 and 15 minutes had quinaldine

residues ranging from 1.49 to 3.90 //g/g at

the 0-hour withdrawal, and were 0.01 //g/g or

less after 8 hours of withdrawal (table 5).

Brook trout were treated for 5.5 minutes at

9 C. and contained a mean quinaldine residue

of 3.13 //g/g at the 0-hour withdrawal and

0.01 //g/g after 8 hours of withdrawal. No

quinaldine residue was detected in any of

these fish after 24 hours of withdrawal.

Northern pike

Northern pike treated with 30 mg/ 1 of quinaldine sulfate for 30 minutes at 7° and 12 C.

were analyzed for quinaldine residue (table o).

Those treated at 7° C. contained a mean quinaldine residue of 4.80 //g/g at the 0-hour

withdrawal and less than 0.01 //g/g of quinaldine residue after 24 hours of withdrawal.

Those treated at 12° C. contained a mean

quinaldine residue of 4.40 //g/g at the 0-hour

withdrawal and 0.17 //g/g after 4 hours of

withdrawal. No samples were available for

the 12° C. treatment with longer than 4 hours

of withdrawal.

analyses.

2 Values less than 0.01 ftg/g are reported as 0.00.

The rainbow trout exposed to the anesthetic 

for 15 minutes at 7° C. contained a mean 

quinaldine residue of 3.53 //g/g at the 0-hour 

withdrawal and 0.17 //g/g after 24 hours of 

withdrawal. Those treated at 12° C. for 5.5

Channel catfish, largemouth bass and bluegill

The warmwater species including channel 

catfish, largemouth bass, and bluegill were 

exposed to the highest concentrations of the 

anesthetic and at the highest temperature, 

19° C., for 30 minutes (table 7). This resulted 

in the highest quinaldine residues encountered
Investigations in Fish Control 50: Bureau of Sport Fisheries and Wildlife

TABLE 5,--Residues of quinaldine in muscle of lake trout 

and brook trout after anesthesia with 25 mg/1 of quinaldine sulfate

TABLE 6. Residues of quinaldine in muscle tissue of 

northern pike following anesthesia with 30 mg/1 of quinaldine sulfate

Withdrawal 

interval

Treatment

Exposure 

( minutes)

Temp.

(°c.)

Mean 

we ight 

(grams)

Residues (i/g/g) 1 

Quinaldine

Mean Range

Withdrawal 

interval

Treatment

Exposure 

(minutes)

Temp. (°c.)

Mean 

weight

(kg)

Residues Ug/g) 1 

Quinaldine

Mean Range

Lake trout

control 0 12 1630 2 Q.OO 0.00

0-hour 5.5 12 1580 2.04- 1.4-9-2.59

1-hour 5.5 12 1270 0.17 0.10-0.28

2-hour 5.5 12 1440 0.11 0.08-0.15

4-hour 5.5 12 1690 0.02 0.01-0.03

8-hour 5,5 12 1500 O.Q1 0.01-0.01

24-hour 5.5 12 1170 0.00 0.00

0-hour 15 12 1430 3.50 3.09-3.90

8-hour 15 12 1620 0.01 0.01-0.02 

24-hour 15 1? 1470 0.00 0.00 

Brook trout 

control 0 9 300 0.00 0.00

0-hour 5.5 9 302 3.13 2.27-3.41

1-hour 5.5 9 344 0.27 0.22-0.30

2-hour 5.5 9 332 0.09 0.06-0.14 

4-hour 5.5 9 297 0.03 0.02-0.04 

8-hour 5.5 9 370 0.01 0.00-0.01 

24-hour 5.5 9 307 0.00 0.00

1 Each mean value represents the average of three analyses. 

2 Vales less than 0.01 j/g/g are reported a? 0.00.

at the 0-hour withdrawal, but after 24 hours

of withdrawal they were 0.01 pg/g or less.

Walleye

Walleye treated with 20 mg/1 of quinaldine 

sulfate for 30 minutes at 7° C. contained a 

mean quinaldine residue of 2.60 //g/g at the 

0-hour withdrawal and 0.04 jtg/g after 6 

hours of withdrawal (table 8). No samples 

were available with longer than 6 hours of 

withdrawal.

control 0

0-hour 30

1-hour 30

2-hour 30

4-hour 30

24-hour 30

7 1.43 2 0.00 0.00

7 1.89 4.80 2.10-8.50

7 1.18 1.10 1.00-1.20

7 1.00 0.51 0.33-0.63

7 1.06 0.06 0.05-0.08

7 1.12 0.00 0.00

control 0 12 1.48 0.00 D.OO

0-hour 30 12 1.91 4.40 2.80-5.4-0

2-hour 30 12 1.63 0.68 0.61-0.76

4- hour 30 12 1.43 0.17 0.05-0.42

1 Each mean value represents the average of three analyses. 

2 Values less than 0.01 fg/g are reported as 0.00.

TABLE 7. Residues of quinaldine in muscle of channel 

catfish, bluegill, and largemouth bass anesthetized 

with quinaldine sulfate for 30 minutes at 19° C.

Withdrawal Treatment 

interval <^SQ4 

(mg/D

Channel

catfish

control 0

0-hour 65

Residues (i/g/g) 1 

Mean Quinaldine 

weight

(grams) 

Mean Range

1,270 2 0.00 0.00

1,320 8.31 7.79-9.34

1-hour 65 1,680 5.55 5.44-5.86 

2-hour 65 680 1.68 1.60-1.76 

4-hour 65 1,320 0.91 0.82-1.00 

6-hour 65 1,090 0.26 0.15-0.40 

24-hour 65 1,680 0.01 0.01-0.01 

See footnotes at end of table.
Sills, Alien, Harman, and Luhning: Residue of Quinaldine in Ten Species of Fish

TABLE 7. Residues of quinaldine in muscle of channel 

catfish, bluegill, and largemouth bass anesthetized 

with quinaldine ^sulfate for 30 minutes at 19° C. 

Continued.

Withdrawal 

interval

Treatment 

QdSO^ 

(mg/D

Mean 

weight 

( grams )

Residues (ftg/g) 1 

Quinaldine

Mean Range

Bluegill

control 0

0-hour 20

1-hour 20

2-hour 20

4 -hour 20

6-hour 20

24 -hour 20

Largemouth 

bass

control 0

0-hour 30

1-hour 30

2 -hour 30

4 -hour 30

6-hour 30

24-hour 30

1 Each mean value repre 

analyses. 

2 Values less than 0.01

115

152

180

135

165

110

112

1,090

1,000

1,000

1,040

590

730

770

0.00 0.00

3.72 3.43-4.07

0.52 0.46-0.63

0.33 0.12-0.61

0.14 0.03-0.22

0.03 0.02-0.04

0.00 0.00-0.01

0.00 0.00

6.07 5.04-7.20

0.76 0.44-1.00

0.20 0.17-0.21

0.05 0.04-0.06

0.05 0.03-0.06

0.00 0.00

sents the average of three 

ftg/g are reported as 0.00.

TABLE 8. Residues of quinaldine in 

following anesthesia with 20 mg/1 

fate at 7° C.

, .,,, ., Treatment Withdrawal

interval (mlnutes)

Walleye

control 0

0-hour 30

1-hour 30

2-hour 30

6 -hour 30

Mean 

weight 

(kg)

0.81

1.32

1.92

0.82

0.82

muscle of walleye 

of quinaldine sulResidues (ftg/g) 1 

Quinaldine

Mean Range

0.00 0.00

2.60 2.20-3.00

1.30 1.10-1.60

0.93 0.70-1.20

0.04 0.02-0.07

1 Each mean value represents the average of three 

analyses.

2 Values less than 0.01 vg/g are reported as 0.00.

DISCUSSION

Residues of quinaldine dissipated rapidly 

from the muscle of all fish in this study. A 

representative curve for disappearance of 

quinaldine residue is shown in figure 1. The 

curves represent the averages of mean values 

obtained on coho salmon, rainbow trout, 

brown trout, brook trout, and lake trout exposed to 25 mg/1 of quinaldine sulfate for 15 

minutes at 12° C., and channel catfish, largemouth bass, and bluegill exposed to 65, 30, 

and 20 mg/1 of quinaldine sulfate, respectively, for a period of 30 minutes at 19° C. 

The regression of the residues in both groups 

of fish is similar to that of MS-222 reported 

by Walker and Schoettger (1967).

The warmwater fish accumulated higher 

concentrations of residues than the salmonids. 

This appears to be directly related to higher 

concentrations of anesthetic, higher temperature, and longer exposure time. Though there 

was wide variation in residue concentrations 

at the 0-hour withdrawal time, residues in all 

fish, except rainbow trout treated at 7° C., 

were at undetectable levels within 24 hours. 

The rainbow trout treated at 7° C., the coldest temperature tested, contained a mean 

quinaldine residue of 3.53 //g/g at the 0-hour 

withdrawal and after 24 hours of withdrawal 

from the anesthetic had fall-en to a mean of 

0.17 ^g/g.

CONCLUSIONS

1. The residues of quinaldine in all the species tested varied considerably at the 

0-hour withdrawal depending on the concentration of anesthetic used, temperature, 

and exposure time. An increase in any of these 

parameters also increased residue concentration at the 0-hour withdrawal time.

2. The residue concentration fell below 0.01 

//g/g after 24 hours of withdrawal in all 

cases, except the rainbow trout treated at 

7°C.

3. The residues of quinaldine dissipated more 

slowly at the lower temperatures. After 

24 hours of withdrawal at 7° C., the rainbow trout still contained an average of 0.17 

f quinaldine residue.
8 Investigations in Fish Control 50: Bureau of Sport Fisheries and Wildlife

6.0

 SALMONIDS

WARMWATER

0

HOURS

Figure 1. Regression of quinaldine residues in muscle tissue of salmonids exposed to quinaldine sulfate at 12° C.

and warmwater fish at 19° C. as a function of time.
Sills, Alien, Harman, and Luhning: Residue of Quinaldine in Ten Species of Fish 9

4. Warmwater species had higher initial quinaldine residues than salmonids.

REFERENCES

Alien, John L.t and Joe B. Sills.

I970a. GUC determination of quinaldine residue 

in fish. Journal of the Association of Official 

Analytical Chemists, vol. 53, p. 20-23.

Alien, John L., and Joe B. Sills.

I970b. U.V. identification and quantitative measurement of quinaldine residues in fish. Journal 

of the Association of Official Analytical Chemists, vol. 53, p. 1170-1171.

Alien, John L0 and Joe B. Sills.

Preparation and properties of quinaldine sulfate, an improved fish anesthetic. U.S. Bureau 

of Sport Fisheries and Wildlife, Investigations 

in Fish Control.

Gilderhus, Philip A.

The efficacy of quinaldine sulfate (QdSO4 ) as 

an anesthetic for freshwater fish. U.S. Bureau 

of Sport Fisheries and Wildlife, Investigations 

in Fish Control.

Luhning, Charles W., and Paul D. Harman.

1971. Sampling of fish muscle for MS-222 and 

quinaldine residues. Journal of the Fisheries 

Research Board of Canada, vol. 28, no. 1, 

p. 113-115.

Sills, Joe B., and Paul D. Harman.

1970. Efficacy and residues of quinaldine sulfate, 

an anesthetic for striped bass (Roccus Saxatilis). 

Proceedings of 24th Annual Conference of the 

Southeastern Association of Game and Fish 

Commissioners, vol. 24, p. 546-549.

Walker, Charles R,, and Richard A. Schoettger.

1967. Residues of MS-222 in four salmonids following anesthesia. U.S. Bureau of Sport Fisheries and Wildlife, Investigations in Fish Control, no. 15, 11 p.

U. S. GOVERNMENT PRINTING OFFICE : 1973 O - 518-291
(Reports 25 through 28 are in one cover.)

25. Field Trials of Antimycin as a Selective Toxicant in Channel Catfish Ponds, by 

Ralph M. Burress and Charles W. Luhning. 1969. 12 p.

26. Laboratory Studies on Antimycin A as a Fish Toxicant, by Bernard L. Berger, Robert E. 

Lennon, and James W. Hogan. 1969. 19 p.

27. Field Trials of Antimycin A as a Fish Toxicant, by Philip A. Gilderhus and Robert E. 

Lennon. 1969. 21 p.

28. Use of Antimycin for Selective Thinning of Sunfish Populations in Ponds, by Ralph M. 

Burress and Charles W. Luhning. 1969. 10 p.

(Reports 29 through 31 are in one cover.)

29. Efficacy of Methylpentynol as an Anesthetic on Four Salmonids, by Robert M. Rowland 

and Richard A. Schoettger. 1969. 11 p.

30. Toxicity of Methylpentynol to Selected Fishes, by Leif L. Marking. 1969. 7 p.

31. Annotated Bibliography on Methylpentynol, by Gerald E. Svendsen. 1969. 7 p.

(Reports 32 through 34 are in one cover.)

32. Toxicity of Hyamine 3500 to Fish, by James W. Hogan. 1969. 9 p.

33. Voidance Time for 23 Species of Fish, by Thomas H. Lane and Howard M. Jackson. 1969. 9 p.

34. Laboratory Studies on Possible Fish-Collecting Aids With Some Toxicities for the Isomers of Cresol, by Robert M. Howland. 1969. 10 p.

35. Toxicology of Thiodan in Several Fish and Aquatic Invertebrates, by Richard A. 

Schoettger. 1970. 31 p.

(Reports 36 through 38 are in one cover.)

36. A Method for Rating Chemicals for Potency Against Fish and Other Organisms, by 

Leif L. Marking. 1970. 8 p.

37. Comparative Toxicity of 29 Nitrosalicylanilides and Related Compounds to Eight Species 

of Fish, by Leif L. Marking and Wayne A. Willford. 1970. 11 p.

38. Toxicity of 33NCS (3'-chloro-3-nitrosalicylanilide) to Freshwater Fish and Sea Lampreys, 

by Leif L. Marking, Everett L. King, Charles R. Walker, and John H. Howell. 1970. 16 p.

(Reports 39 and 40 are in one cover.)

39. Effects of Antimycin A on Tissue Respiration of Rainbow Trout and Channel Catfish, by 

Richard A. Schoettger and Gerald E. Svendsen. 1970. 10 p.

40. A Resume on Field Applications of Antimycin A to Control Fish, by Robert E. Lennon 

and Bernard L. Berger. 1970. 19 p.

(Reports 41 through 43 are in one cover.)

41. Identification of MS-222 Residues in Selected Fish Tissues by Thin Layer Chromatography, 

by John L. Alien, Charles W. Luhning, and Paul D. Harman. 1970. 7 p.

42. Dynamics of MS-222 in the Blood and Brain of Freshwater Fishes During Anesthesia, by 

Joseph B. Hunn. 1970. 8 p.

43. Effect of MS-222 on Electrolyte and Water Content in the Brain of Rainbow Trout, by 

Wayne A. Willford. 1970. 7 p.

44. A Review of Literature on TFM (3-trifluormethyl-4-nitrophenol) as a Lamprey Larvicide, 

by Rosalie A. Schnick. 1972. 31 p.

(Reports 45 and 46 are in one cover.)

45. Residues of MS-222 in Northern Pike, Muskellunge, and Walleye, by John L. Alien, 

Charles W. Luhning, and Paul D. Harman. 1972. 8 p.

46. Methods of Estimating the Half-Life of Biological Activity of Toxic Chemicals in Water, 

by Leif L. Marking. 1972. 9 p.
As the Nation's principal conservation agency, the Department 

of the Interior has basic responsibilities for water, fish, wildlife, 

mineral, land, park, and recreational resources. Indian and Territorial affairs are other major .concerns of this department of 

natural resources.

The Department works to assure the wisest choice in managing 

all our resources so that each shall make its full contribution to 

a better United States now and in the future.

UNITED STATES 

DEPARTMENT OF THE INTERIOR

FISH AND WILDLIFE SERVICE

BUREAU OF SPORT FISHERIES AND WILDLIFE 

WASHINGTON. D. C. 2O24O

POSTAGE AND FEES PAID 

U.S. DEPARTMENT OF THE INTERIOR

INT 423