U.S. Department of the Interior

U.S. Geological Survey

Open-File Report 2012–1268

Prepared in collaboration with the Missouri Department of Conservation

Concentrations of Elements in Fish Fillets, Fish Muscle 

Plugs, and Crayfish from the 2011 Missouri Department 

of Conservation General Contaminant Monitoring 

Program

Concentrations of Elements in Fish Fillets, 

Fish Muscle Plugs, and Crayfish from the 

2011 Missouri Department of Conservation 

General Contaminant Monitoring Program

By Thomas W. May, Michael J. Walther, William G. Brumbaugh, and Michael J. 

McKee

Prepared in collaboration with the Missouri Department of Conservation

Open-File Report 2012–1268

U.S. Department of the Interior

U.S. Geological Survey
U.S. Department of the Interior

KEN SALAZAR, Secretary

U.S. Geological Survey

Marcia K. McNutt, Director

U.S. Geological Survey, Reston, Virginia: 2013

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Suggested citation:

May, T.W., Walther, M.J., Brumbaugh, W.G., and McKee, M.J., 2013, Concentrations of elements in fish fillets, fish 

muscle plugs, and crayfish from the 2011 Missouri Department of Conservation general contaminant monitoring program: U.S. Geological Survey Open-File Report 2012–1268, 12 p. 
iii

Contents

Abstract...........................................................................................................................................................1

Introduction.....................................................................................................................................................1

Sampling History............................................................................................................................................1

Methods...........................................................................................................................................................2

Sites and Sample Collection ...............................................................................................................2

Homogenization and Lyophilization ...................................................................................................2

Chemical Preparation ..........................................................................................................................2

Instrumental Analysis...........................................................................................................................2

Quality Control................................................................................................................................................2

Results .............................................................................................................................................................2

 Quality-Control Results ..............................................................................................................................11

References Cited..........................................................................................................................................12

Tables

1. Missouri collection sites for fish fillets, fish muscle plugs, and crayfish 

from the 2011 Missouri Department of Conservation General Contaminant 

Monitoring Program.....................................................................................................................3

2. Percent moisture and dry weight concentrations of calcium, zinc, cadmium, 

lead, and lead/calcium molar ratios in Missouri Department of Conservation 

2011 General Contaminant Monitoring Program fish fillet, fish muscle plug, 

and crayfish samples ...................................................................................................................4

3. Percent moisture and wet weight concentrations of calcium, zinc, cadmium, 

and lead in Missouri Department of Conservation 2011 General Contaminant 

Monitoring Program fish fillet, fish muscle plug, and crayfish samples .............................6

4. Concentrations of total mercury in fish fillets, fish muscle plugs, and crayfish 

tissues.............................................................................................................................................8
iv

Conversion Factors

Multiply By To obtain

Length

millimeter (mm) 0.03937 inch (in.)

micrometer 0.0000393 inch (in.)

Volume

liter (L) 33.82 ounce, fluid (fl. oz)

milliliter (mL) .034 ounce, fluid (fl. oz)

Mass

gram (g) 0.03527 ounce, avoirdupois (oz)

milligram (mg) .000035 ounce, avoirdupois (oz)

microgram (μg) 0.000000035 ounce, avoirdupois (oz)

Temperature in degrees Celsius (°C) may be converted to degrees Fahrenheit (°F) as follows: 

°F=(1.8×°C)+32

Concentrations of chemical constituents in water are given in nanograms per milliliter (ng/mL).

Concentrations of chemical constituents in solid materials are given in either micrograms per 

gram (μg/g) dry weight or μg/g wet weight.
Concentrations of Elements in Fish Fillets, Fish Muscle 

Plugs, and Crayfish from the 2011 Missouri Department of 

Conservation General Contaminant Monitoring Program

By Thomas W. May1, Michael W. Walther1, William G. Brumbaugh1, and Michael J. McKee2

1

U.S. Geological Survey

2

Missouri Department of Conservation

Abstract

This report presents the results of a contaminant monitoring survey conducted annually by the Missouri Department 

of Conservation to examine the levels of selected elemental 

contaminants in fish fillets, fish muscle plugs, and crayfish. 

Fillet samples of yellow bullhead (Ameiurus natalis), golden 

redhorse (Moxostoma erythrurum), longear sunfish (Lepomis 

megalotis), and channel catfish (Ictalurus punctatus) were 

collected from six sites as part of the Missouri Department of 

Conservation’s Fish Contaminant Monitoring Program. Fish 

dorsal muscle plugs were collected from largemouth bass 

(Micropterus salmoides) at eight of the sites, and crayfish from 

two sites. Following preparation and analysis of the samples, 

highlights of the data were as follows: cadmium and lead 

residues were most elevated in crayfish tissue samples from 

the Big River at Cherokee Landing, with 1 to 8 micrograms 

per gram dry weight and 22 to 45 micrograms per gram dry 

weight, respectively. Some dorsal muscle plugs from largemouth bass collected from Clearwater Lake, Lake St. Louis, 

Noblett Lake, Hazel Creek Lake, and Harrison County Lake 

contained mercury residues (1.7 to 4.7 micrograms per gram 

dry weight) that exceeded the U.S. Environmental Protection 

Agency Water Quality Criterion of 1.5 micrograms per gram 

dry weight of fish tissue (equivalent to 0.30 micrograms per 

gram wet weight).

Introduction

The Missouri Department of Conservation (MDC) 

initiated long-term statewide fish monitoring of environmental contaminants in 1984 with the objective of selecting 

predator and bottom dwelling species annually from each of 

20 to 30 lakes and streams across Missouri to characterize 

concentrations of targeted metals and other chemical contaminants. Actual sites monitored each year vary based on 

data needs, budgets, and personnel resources. Emphasis is on 

human health effects from recreational and sport fishing, so 

study components include fish fillets, composite fillet samples, 

and sample replication at each site. The MDC has requested 

the assistance of the U.S. Geological Survey (USGS) for this 

monitoring program because of past experience with aquatic 

biota monitoring projects and expertise in the preparation and 

analysis of aquatic biota for elemental contaminants. For more 

detailed information on the overall study design or specific 

sample information, please contact the Missouri Department 

of Conservation in Columbia, Missouri (http://mdc.mo.gov/

regions/central).

Sampling History

A shipment of 27 whole-body fish, 25 fish fillets, 48 fish 

muscle plugs, and 37 crayfish tissues was received by USGS 

personnel on December 7, 2011. The samples included skinless fillets collected from yellow bullhead, golden redhorse, 

longear sunfish, and channel catfish to reflect the form of fish 

tissue customarily consumed by anglers. Dorsal fish muscle 

plugs were collected from largemouth bass for purposes of 

assessing mercury accumulation. Crayfish tissues were collected for assessing lead accumulation. Upon receipt, the 

shipment was assigned USGS batch number 1974 and sample 

identifications (IDs) 55878-55987. All samples had been 

stored frozen at -20 degrees Celsius (o C) since collection at 

the MDC’s Resource Science Center in Columbia, Missouri, 

and were delivered by MDC personnel. Requested analyses 

included zinc (Zn), cadmium (Cd), mercury (Hg), and lead 

(Pb). Calcium (Ca) also was analyzed in an effort to explain 

Pb variability (Schmitt and Finger, 1987). Fish fillet samples 

were variable in the way they were obtained, and the fillet 

technique may have resulted in different amounts of tissue 

extracted and, thus, may have varying amounts of calcium-rich 

bone fragments that can be comparatively high in Pb.
2 Concentrations of Elements in Fish Fillets, Fish Muscle Plugs, and Crayfish from the 2011 Contaminant Monitoring Program

Methods

Sites and Sample Collection

In 2011, 16 sites (table 1) were selected for sampling as 

part of the MDC General Contaminant Monitoring Program 

(GCMP). The 2011 collection consisted of yellow bullhead 

(Ameiurus natalis), golden redhorse (Moxostoma erythrurum), 

longear sunfish (Lepomis megalotis), and channel catfish 

(Ictalurus punctatus). Besides fish fillet samples collected in 

2011, fish dorsal muscle plugs were collected from largemouth 

bass (Micropterus salmoides), and tissues [tail shell, tail-meat, 

and carcass (crayfish remains after tail meat was removed or 

extracted)] were collected from crayfish. 

Homogenization and Lyophilization

GCMP fillet samples were chopped and minced with 

a titanium meat cleaver on a cleaned polypropylene cutting 

board and then lyophilized. Fish muscle plugs and crayfish tissues (tail meat and non tail meat) were lyophilized as received. 

After lyophilization, fish fillet samples were hand-kneaded in 

a plastic (polyethylene) bag or crushed with a rolling pin in a 

plastic bag to achieve a coarse powder consistency, whereas 

crayfish tissues were placed in a glass vial and ground with a 

glass rod. All dried and ground products were stored at room 

temperature in a 40-milliliter (mL) glass vial in a nitrogen 

desiccator. 

Chemical Preparation

To prepare fish samples for analysis of Ca, Zn, Cd, and 

Pb, a dried sample of approximately 0.25 grams (g) was 

heated with 6mL of nitric acid in a sealed high-pressure 

Teflon® vessel in a laboratory microwave oven. The cooled 

digestate liquid was transferred into a 125-mL polyethylene 

bottle with ultrapure water [specific resistance greater than (>) 

10 megOhms per centimeter (megOhm/cm)] and diluted to 

a final weight of 101.5 g. Final acid matrix was 6 percent by 

volume concentrated nitric acid. For the determination of Hg 

in fish samples, there was no chemical preparation (digestion) 

because the dried sample was decomposed thermally during 

instrumental analysis (see Instrumental Analysis section). 

Instrumental Analysis

Calcium, Zn, Cd, and Pb analyses were conducted using 

a PE/SCIEX Elan 6000® inductively coupled plasma-mass 

spectrometer (ICP-MS), which was set up in “Standard Mode” 

and optimized according to the manufacturer’s specifications. 

Samples were delivered automatically to the ICP-MS by 

means of a software-controlled CETAC ASD-500 autosampler/autodiluter system. All sample digestates were analyzed 

with a 10-fold predilution by autodiluter. 

The ICP-MS quantitative method was designed to 

determine the following masses: 44Ca and 48Ca, 60Zn and 68Zn, 111Cd and 114Cd, and Pb as the sum of three masses 

(206Pb+207Pb+208Pb). The internal standards were scandium 

(Sc) at 10 nanograms per milliliter (ng/mL), rhodium (Rh; 

10 ng/mL), and bismuth (Bi; 10 ng/mL), which were metered 

into the sample line via peristaltic pump. Calibration standards for analyses were as follows: Ca - 2500, 5000, and 

10,000 ng/mL; Zn - 75, 150, and 300 ng/mL; Pb - 5, 10, 20, 

and 40 ng/mL; and Cd - 1.5, 3.0, 6.0, and 12 ng/mL. During 

the actual analysis, any digestate concentration greater than the 

upper calibration standard for any element was automatically 

diluted 10-fold serially until its concentration was below this 

level. Where multiple masses for an element were measured, 

the concentration reported was based on the mass exhibiting 

least interferences, which were as follows: 44Ca, 60Zn, 114Cd , 

and Pb as the sum of three masses 206Pb+207Pb+208Pb).

Mercury was determined with a Milestone DMA-80 

analyzer equipped with an automated sample carousel. With 

this method, a dried fish sample [40 to 60 milligrams (mg)] 

was combusted in a stream of oxygen. All Hg in the sample 

was volatilized and trapped by amalgamation on a gold substrate, and was thermally desorbed and quantitated by atomic 

absorption spectrophotometry (U. S. Environmental Protection 

Agency, 1998). 

Quality Control

The samples were digested and analyzed in two groups 

or batches for Ca, Zn, Cd, and Pb, and four batches for Hg. 

The quality-control incorporated in the digestion stage of the 

samples (for subsequent ICP-MS analysis) included digestion 

blanks, reference materials, replicates, and spikes. For the 

determination of Ca, Zn, Cd, and Pb by ICP-MS, instrumental 

quality control included calibration checks, laboratory control 

solutions, duplicate digestate analysis, analysis spikes, and 

interference checks (dilution percent difference and a synthetic interference solution). Quality control for Hg included 

blanks, independent calibration verification checks, replicates, 

pre-combustion spikes, and tissue reference materials. All 

quality-control results were tabulated to provide an overview 

of quality assurance and to facilitate interpretation.

Results 

Percent moisture, concentrations in micrograms per gram 

(μg/g) dry weight of Ca, Zn, Cd, and Pb, and molar ratios 

(fillet samples only) of [Pb/Ca] (1 x 10-6) for the fish fillet and 

crayfish tissues are presented in table 2. To facilitate comparison with any regulatory guidelines, concentrations of Ca, Zn, 

Cd, and Pb are presented for these matrices in micrograms per 

gram wet weight in table 3. Concentrations of total mercury 

in micrograms per gram dry and wet weight in fish fillets, fish 
Results 3

Table 1. Missouri collection sites for fish fillets, fish muscle plugs, and crayfish from the 2011 

Missouri Department of Conservation General Contaminant Monitoring Program.

Species and Common Name Sites Sample Type

Ameiurus natalis Mound Branch at Paxton, Missouri Fillet

Yellow Bullhead

Moxostoma erythrurum Big River at House Springs Fillet

Golden Redhorse Meramec River at Allenton Access Fillet

Meramec River at Route 66 State Park Fillet

Lepomis megalotis Meramec River at Allenton Access Fillet

Longear Sunfish Big River at House Springs Fillet

Meramec River at Route 66 State Park Fillet

Ictalurus punctatus Wakonda State Park at Agate Lake Fillet

Channel Catfish Wakonda State Park at Wakonda Lake Fillet

Micropterus salmoides Lake of the Ozarks at Niangua Arm Plug

Largemouth Bass Longview Lake Plug

Stockton Lake at Big Sac Arm Plug

Clearwater Lake Plug

Lake St. Louis Plug

Noblett Lake Plug

Hazel Creek Lake Plug

Harrison County Lake Plug

Crayfish species Big River at Cherokee Landing Tail meat

Non tail meat

Shoal Creek 0.5 mile North of I-44 Bridge Tail meat

Non tail meat

Tail shell

muscle plugs, and crayfish tissues are presented in table 4. For 

this report all sample and quality-control data are discussed in 

terms of dry weight results only. 

Calcium concentrations were variable among fillet 

samples; concentrations were generally within a factor of two 

or three among golden redhorse, but increased to a factor of 

seven in longear sunfish (table 2). Such variation presumably was because of variable bone content in the fillets and 

undoubtedly was affected by significant variations in fillet 

preparation techniques as well as by the fish species. For 

example, catostomids possess numerous tiny intermuscular 

bones. Accordingly, fillets from some species (golden redhorse and longear sunfish) contained higher Ca concentrations 

than other species (catfish). Although Ca normally is not a 

target analyte, fillet Ca concentrations are useful when target 

analytes include those that markedly accumulate in bone (for 

example, Pb). Thus, measurements of Ca can help explain 

high variation in Pb concentrations for individual samples 

that included variable amounts of Ca-rich tissue (Schmitt and 

Finger, 1987). Concentrations of Ca in crayfish tail-meat were 

similar to those of fish fillets, but concentrations in crayfish 

carcass remains and shell samples were some 100 fold higher. 

Zinc concentrations were quite uniform in fillet samples 

among the different species of fish, ranging from 20 to 31 μg/g 

dry weight. Concentrations of Zn (μg/g dry weight) in crayfish 

tissues were lowest in tail shell samples (17 to 25), but three 

to six fold higher in tail meat and carcass samples (71 to 134). 

Cadmium concentrations (μg/g dry weight) were less than 

0.1 in most fish fillet samples (72 percent of sample set) and 

ranged from 0.1 to 0.26 in remaining fillet samples. Cadmium 
4 Concentrations of Elements in Fish Fillets, Fish Muscle Plugs, and Crayfish from the 2011 Contaminant Monitoring Program Table 2. Percent moisture and dry weight concentrations of calcium, zinc, cadmium, lead, and lead/calcium molar ratios in Missouri Department of Conservation 2011 General Contaminant Monitoring Program fish fillet, fish muscle plug, and crayfish samples. [USGS, U.S. Geological Survey; ID, identification; MDC, Missouri Department of Conservation; Ca, calcium; μg/g, micrograms per gram dry weight; Zn, zinc; Cd, cadmium; Pb, lead; <, less than; bold and italicized values are greater than the method detection limit but less than the method quantitation limit and have higher uncertainty] USGS ID MDC ID Biota common name Matrix Percent moisture Ca μg/g Zn μg/g Cd μg/g Pb μg/g Pb/Ca molar ratio (1X10-6) 55881 2011-723-240-1 Yellow Bullhead Fish fillet 81.9 776 31.3 <0.012 0.10 25 55878 2011-056-062-1 Golden Redhorse Fish fillet 81.0 4,960 20.9 0.034 1.50 59 55879 2011-056-062-2 Golden Redhorse Fish fillet 81.5 4,690 23.8 0.04 1.39 57 55880 2011-056-062-3 Golden Redhorse Fish fillet 79.9 3,170 21.0 0.025 0.82 50 55882 2011-724-062-1 Golden Redhorse Fish fillet 80.7 3,230 24.8 0.032 0.12 7.2 55883 2011-724-062-2 Golden Redhorse Fish fillet 80.5 1,340 21.2 0.075 0.037 5.3 55884 2011-724-062-3 Golden Redhorse Fish fillet 80.1 2,270 24.0 0.26 0.087 7.4 55885 2011-725-062-1 Golden Redhorse Fish fillet 80.8 4,640 25.1 0.19 0.37 15 55886 2011-725-062-2 Golden Redhorse Fish fillet 81.5 3,050 21.2 0.10 0.21 13 55887 2011-725-062-3 Golden Redhorse Fish fillet 80.8 3,190 22.3 0.093 0.21 13 55888 2011-724-420-1 Longear Sunfish Fish fillet 81.4 818 20.4 0.047 0.020 4.7 55889 2011-724-420-2 Longear Sunfish Fish fillet 82.8 1,440 23.6 0.11 0.023 3.1 55890 2011-724-420-3 Longear Sunfish Fish fillet 81.1 1,820 22.8 0.14 0.057 6.1 55891 2011-056-420-1 Longear Sunfish Fish fillet 81.2 3,910 29.8 0.038 0.81 40 55892 2011-056-420-2 Longear Sunfish Fish fillet 80.2 6,260 26.3 0.028 1.11 34 55893 2011-056-420-3 Longear Sunfish Fish fillet 78.9 5,550 25.7 0.041 1.12 39 55900 2011-725-420-1 Longear Sunfish Fish fillet 81.5 1,920 22.6 0.14 0.19 19 55901 2011-725-420-2 Longear Sunfish Fish fillet 81.8 1,690 24.2 0.15 0.18 21 55902 2011-725-420-3 Longear Sunfish Fish fillet 81.5 834 24.5 0.066 0.052 12 55894 2011-459-230-1 Channel Catfish Fish fillet 83.8 590 27.4 <0.012 0.069 23 55895 2011-459-230-2 Channel Catfish Fish fillet 84.5 604 31.4 <0.012 0.033 11 55896 2011-459-230-3 Channel Catfish Fish fillet 82.7 546 26.1 <0.012 0.037 13 55897 2011-514-230-1 Channel Catfish Fish fillet 78.1 489 20.8 <0.012 0.023 9.1 55898 2011-514-230-2 Channel Catfish Fish fillet 78.3 527 24.0 <0.012 0.029 11 55899 2011-514-230-3 Channel Catfish Fish fillet 80.0 538 24.9 <0.012 0.018 6.5 55952 2011-134-609-1-S Crayfish species Carcassa 73.8 247,000 70.2 4.78 21.9 17

55954 2011-134-609-2-S Crayfish species Carcass 71.4 166,000 93.8 5.74 29.0 3455956 2011-134-609-3-S Crayfish species Carcass 71.3 115,000 115 3.03 31.8 5355958 2011-134-609-4-S Crayfish species Carcass 74.4 255,000 73.8 4.03 28.9 22
Results 

5

Table 2. Percent moisture and dry weight concentrations of calcium, zinc, cadmium, lead, and lead/calcium molar ratios in Missouri Department of Conservation 2011 General Contaminant Monitoring Program fish fillet, fish muscle plug, and crayfish samples.—Continued

[USGS, U.S. Geological Survey; ID, identification; MDC, Missouri Department of Conservation; Ca, calcium; μg/g, micrograms per gram dry weight; Zn, zinc; Cd, cadmium; Pb, lead; <, less than; bold and italicized values are greater than the method detection limit but less than the method quantitation limit and have higher uncertainty] 

 USGS

ID

MDC

ID

Biota

common name

Matrix Percent moisture Ca μg/g Zn μg/g Cd μg/g Pb μg/g Pb/Ca molar ratio (1X10-6)

55960 2011-134-609-5-S Crayfish species Carcass 80.0 182,000 92.2 7.79 37.5 4055962 2011-134-609-6-S Crayfish species Carcass 72.1 151,000 101 5.50 40.6 5255964 2011-134-609-7-S Crayfish species Carcass 77.6 173,000 77.4 5.82 27.9 3156227 2011-134-609-M Compositeb Crayfish species Tail meat 83.2c 3,550 116 1.06 44.9 2,450

55965 2011-726-609-1-M Crayfish species Tail meat 85.6 1,560 79.1 0.027 0.29 36

55966 2011-726-609-1-S Crayfish species Carcass 75.9 133,000 134 0.46 0.59 0.955967 2011-726-609-2-M Crayfish species Tail meat 82.6 2,370 69.1 0.02 0.27 22

55968 2011-726-609-2-S Crayfish species Carcass 70.1 164,000 75.6 0.40 0.72 0.8

55969 2011-726-609-3-M Crayfish species Tail meat 78.7 1,210 78.4 0.046 0.26 42

55970 2011-726-609-3-S Crayfish species Carcass 65.6 127,000 94.5 0.60 2.43 3.755971 2011-726-609-4-M Crayfish species Tail meat 79.1 1,270 76.8 0.028 0.18 27

55972 2011-726-609-4-S Crayfish species Carcass 68.4 114,000 99.7 0.43 2.00 3.455973 2011-726-609-5-M Crayfish species Tail meat 78.8 2,090 81.2 0.027 0.28 26

55974 2011-726-609-5-S Crayfish species Carcass 65.4 124,000 129 0.50 3.33 5.255975 2011-726-609-6-M Crayfish species Tail meat 85.3 2,720 85.1 0.017 0.18 13

55976 2011-726-609-6-S Crayfish species Carcass 73.1 172,000 83.6 0.20 0.70 0.855977 2011-726-609-7-M Crayfish species Tail meat 81.6 3,670 70.7 0.028 0.17 9.0

55978 2011-726-609-7-S Crayfish species Carcass 67.5 128,000 112 0.31 1.10 1.755979 2011-726-609-8-M Crayfish species Tail meat 87.7 2,570 98.7 0.33 4.74 357

55980 2011-726-609-8-S Crayfish species Carcass 74.2 144,000 102 0.24 1.06 1.455981 2011-726-609-8-T Crayfish species Tail shell 72.2 239,000 17.2 0.029 0.69 0.655982 2011-726-609-9-M Crayfish species Tail meat 86.3 4,170 82.1 0.09 1.61 75

55983 2011-726-609-9-S Crayfish species Carcass 69.8 112,000 98.3 0.23 0.93 1.655984 2011-726-609-9-T Crayfish species Tail shell 68.1 165,000 24.9 0.02 0.86 1.055985 2011-726-609-10-M Crayfish species Tail meat 86.5 2,890 93.4 0.19 2.78 186

55986 2011-726-609-10-S Crayfish species Carcass 69.5 130,000 101 0.23 0.95 1.455987 2011-726-609-10-T Crayfish species Tail shell 68.9 228,000 20.6 0.042 1.24 1.1

aCarcass is defined as crayfish remains after tail meat has been removed or extracted.bBecause of insufficient biomass in submitted individual samples, this sample is a composite of seven crayfish tail meat samples collected from the Big River at Cherokee Landing (55951, 55953, 

55955, 55957, 55959, 55961, 55963).

cAverage moisture for all crayfish tail meat samples used as moisture value for this tail meat composite.
6 Concentrations of Elements in Fish Fillets, Fish Muscle Plugs, and Crayfish from the 2011 Contaminant Monitoring Program Table 3. Percent moisture and wet weight concentrations of calcium, zinc, cadmium, and lead in Missouri Department of Conservation 2011 General Contaminant Monitoring Program fish fillet, fish muscle plug, and crayfish samples. [USGS, U.S. Geological Survey; MDC, Missouri Department of Conservation; ID, identification; Ca, calcium; μg/g, micrograms per gram wet weight; Zn, zinc; Cd, cadmium; Pb, lead; <, less than; bold and italicized values are greater than the method detection limit but less than the method quantita- tion limit and have higher uncertainty] USGS ID MDC ID Biota common name Matrix Percent moisture Ca μg/g Zn μg/g Cd μg/g Pb μg/g 55878 2011-056-062-1 Golden Redhorse Fish fillet 81.0 941 4.0 0.006 0.28 55879 2011-056-062-2 Golden Redhorse Fish fillet 81.5 869 4.4 0.007 0.26 55880 2011-056-062-3 Golden Redhorse Fish fillet 79.9 638 4.2 0.005 0.17 55881 2011-723-240-1 Yellow Bullhead Fish fillet 81.9 140 5.7 <0.003 0.018 55882 2011-724-062-1 Golden Redhorse Fish fillet 80.7 623 4.8 0.006 0.023 55883 2011-724-062-2 Golden Redhorse Fish fillet 80.5 261 4.1 0.015 0.007 55884 2011-724-062-3 Golden Redhorse Fish fillet 80.1 452 4.8 0.052 0.017 55885 2011-725-062-1 Golden Redhorse Fish fillet 80.8 891 4.8 0.036 0.071 55886 2011-725-062-2 Golden Redhorse Fish fillet 81.5 564 3.9 0.018 0.039 55887 2011-725-062-3 Golden Redhorse Fish fillet 80.8 612 4.3 0.018 0.040 55888 2011-724-420-1 Longear Sunfish Fish fillet 81.4 152 3.8 0.009 0.004 55889 2011-724-420-2 Longear Sunfish Fish fillet 82.8 247 4.0 0.019 0.004 55890 2011-724-420-3 Longear Sunfish Fish fillet 81.1 345 4.3 0.027 0.011 55891 2011-056-420-1 Longear Sunfish Fish fillet 81.2 733 5.6 0.007 0.15 55892 2011-056-420-2 Longear Sunfish Fish fillet 80.2 1,240 5.2 0.006 0.22 55893 2011-056-420-3 Longear Sunfish Fish fillet 78.9 1,170 5.4 0.009 0.24 55900 2011-725-420-1 Longear Sunfish Fish fillet 81.5 356 4.2 0.026 0.035 55901 2011-725-420-2 Longear Sunfish Fish fillet 81.8 307 4.4 0.027 0.033 55902 2011-725-420-3 Longear Sunfish Fish fillet 81.5 154 4.5 0.012 0.010 55894 2011-459-230-1 Channel Catfish Fish fillet 83.8 95 4.4 <0.003 0.011 55895 2011-459-230-2 Channel Catfish Fish fillet 84.5 93 4.9 <0.004 0.005 55896 2011-459-230-3 Channel Catfish Fish fillet 82.7 94 4.5 <0.005 0.006 55897 2011-514-230-1 Channel Catfish Fish fillet 78.1 107 4.6 <0.006 0.005 55898 2011-514-230-2 Channel Catfish Fish fillet 78.3 115 5.2 <0.007 0.006 55899 2011-514-230-3 Channel Catfish Fish fillet 80.0 107 5.0 <0.008 0.004 55952 2011-134-609-1-S Crayfish species Carcassa 73.8 64,700 18. 1.25 5.74 55954 2011-134-609-2-S Crayfish species Carcass 71.4 47,400 27. 1.64 8.29

55956 2011-134-609-3-S Crayfish species Carcass 71.3 33,100 33. 0.87 9.14

55958 2011-134-609-4-S Crayfish species Carcass 74.4 65,300 19. 1.03 7.40

55960 2011-134-609-5-S Crayfish species Carcass 80.0 36,400 18. 1.56 7.50
Results 

7

Table 3. Percent moisture and wet weight concentrations of calcium, zinc, cadmium, and lead in Missouri Department of Conservation 2011 General Contaminant Monitoring Program fish fillet, fish muscle plug, and crayfish samples.—Continued[USGS, U.S. Geological Survey; MDC, Missouri Department of Conservation; ID, identification; Ca, calcium; μg/g, micrograms per gram wet weight; Zn, zinc; Cd, cadmium; Pb, lead; <, less than; bold and italicized values are greater than the method detection limit but less than the method quantitation limit and have higher uncertainty] 

 USGS

ID

MDC

ID

Biota

common name

Matrix Percent moisture Ca μg/g Zn μg/g Cd μg/g Pb μg/g

55962 2011-134-609-6-S Crayfish species Carcass 72.1 42,100 28. 1.53 11.355964 2011-134-609-7-S Crayfish species Carcass 77.6 38,700 17. 1.30 6.25

56227 2011-134-609-M Compositeb Crayfish species Tail meat 83.2c 596 19. 0.18 7.54

55965 2011-726-609-1-M Crayfish species Tail meat 85.6 225 11. 0.004 0.042

55966 2011-726-609-1-S Crayfish species Carcass 75.9 32,100 32. 0.11 0.1455967 2011-726-609-2-M Crayfish species Tail meat 82.6 412 12. 0.003 0.047

55968 2011-726-609-2-S Crayfish species Carcass 70.1 49,100 23. 0.12 0.22

55969 2011-726-609-3-M Crayfish species Tail meat 78.7 258 17. 0.010 0.055

55970 2011-726-609-3-S Crayfish species Carcass 65.6 43,700 32. 0.21 0.84

55971 2011-726-609-4-M Crayfish species Tail meat 79.1 266 16. 0.006 0.038

55972 2011-726-609-4-S Crayfish species Carcass 68.4 36,000 31. 0.14 0.63

55973 2011-726-609-5-M Crayfish species Tail meat 78.8 444 17. 0.006 0.059

55974 2011-726-609-5-S Crayfish species Carcass 65.4 42,900 45. 0.17 1.15

55975 2011-726-609-6-M Crayfish species Tail meat 85.3 400 13. 0.002 0.026

55976 2011-726-609-6-S Crayfish species Carcass 73.1 46,200 22. 0.054 0.19

55977 2011-726-609-7-M Crayfish species Tail meat 81.6 677 13. 0.005 0.031

55978 2011-726-609-7-S Crayfish species Carcass 67.5 41,500 36. 0.10 0.36

55979 2011-726-609-8-M Crayfish species Tail meat 87.7 317 12. 0.041 0.59

55980 2011-726-609-8-S Crayfish species Carcass 74.2 37,100 26. 0.062 0.27

55981 2011-726-609-8-T Crayfish species Tail shell 72.2 66,500 4.8 0.008 0.19

55982 2011-726-609-9-M Crayfish species Tail meat 86.3 570 11. 0.013 0.22

55983 2011-726-609-9-S Crayfish species Carcass 69.8 33,800 30. 0.069 0.28

55984 2011-726-609-9-T Crayfish species Tail shell 68.1 52,700 8.0 0.006 0.27

55985 2011-726-609-10-M Crayfish species Tail meat 86.5 389 13. 0.026 0.37

55986 2011-726-609-10-S Crayfish species Carcass 69.5 39,600 31. 0.070 0.29

55987 2011-726-609-10-T Crayfish species Tail shell 68.9 70,800 6.4 0.013 0.39

aCarcass is defined as crayfish remains after tail meat has been removed or extracted.bBecause of insufficient biomass in submitted individual samples, this sample is a composite of 7 crayfish tail meat samples collected from the Big River at Cherokee Landing (55951, 55953, 

55955, 55957, 55959, 55961, 55963). 

cAverage moisture for all crayfish tail meat samples used as moisture value for this tail meat composite..
8 Concentrations of Elements in Fish Fillets, Fish Muscle Plugs, and Crayfish from the 2011 Contaminant Monitoring Program Table 4. Concentrations of total mercury in fish fillets, fish muscle plugs, and crayfish tissues. [USGS, U.S. Geological Survey; MDC, Missouri Department of Conservation; Hg, mercury; μg/g, micrograms per gram; wet weight concentrations estimated assuming 80 percent moisture]. USGS ID MDC ID Site location Biota common name Matrix Hg μg/g dry weight Hg μg/g wet weight 55878 2011-056-062-1 Big River at House Springs Golden Redhorse Fish fillet 0.21 0.042 55879 2011-056-062-2 Big River at House Springs Golden Redhorse Fish fillet 0.29 0.059 55880 2011-056-062-3 Big River at House Springs Golden Redhorse Fish fillet 0.18 0.036 55881 2011-723-240-1 Mound Branch at Paxton, Missouri Yellow Bullhead Fish fillet 0.74 0.15 55882 2011-724-062-1 Meramec River at Allenton Access Golden Redhorse Fish fillet 0.55 0.11 55883 2011-724-062-2 Meramec River at Allenton Access Golden Redhorse Fish fillet 0.81 0.16 55884 2011-724-062-3 Meramec River at Allenton Access Golden Redhorse Fish fillet 0.06 0.012 55885 2011-725-062-1 Meramec River at Route 66 State Park Golden Redhorse Fish fillet 0.61 0.12 55886 2011-725-062-2 Meramec River at Route 66 State Park Golden Redhorse Fish fillet 0.50 0.10 55887 2011-725-062-3 Meramec River at Route 66 State Park Golden Redhorse Fish fillet 0.47 0.093 55888 2011-724-420-1 Meramec River at Allenton Access Longear Sunfish Fish fillet 0.26 0.052 55889 2011-724-420-2 Meramec River at Allenton Access Longear Sunfish Fish fillet 0.48 0.10 55890 2011-724-420-3 Meramec River at Allenton Access Longear Sunfish Fish fillet 0.22 0.044 55891 2011-056-420-1 Big River at House Springs Longear Sunfish Fish fillet 0.16 0.032 55892 2011-056-420-2 Big River at House Springs Longear Sunfish Fish fillet 0.15 0.029 55893 2011-056-420-3 Big River at House Springs Longear Sunfish Fish fillet 0.12 0.025 55894 2011-459-230-1 Wakonda State Park at Agate Lake Channel Catfish Fish fillet 1.14 0.23 55895 2011-459-230-2 Wakonda State Park at Agate Lake Channel Catfish Fish fillet 0.41 0.081 55896 2011-459-230-3 Wakonda State Park at Agate Lake Channel Catfish Fish fillet 1.30 0.26 55897 2011-514-230-1 Wakonda State Park at Agate Lake Channel Catfish Fish fillet 0.17 0.034 55898 2011-514-230-2 Wakonda State Park at Agate Lake Channel Catfish Fish fillet 0.32 0.064 55899 2011-514-230-3 Wakonda State Park at Agate Lake Channel Catfish Fish fillet 0.11 0.023 55900 2011-725-420-1 Meramec River at Route 66 State Park Longear Sunfish Fish fillet 0.29 0.058 55901 2011-725-420-2 Meramec River at Route 66 State Park Longear Sunfish Fish fillet 0.34 0.069 55902 2011-725-420-3 Meramec River at Route 66 State Park Longear Sunfish Fish fillet 0.30 0.060 55903 2011-025-406-1 Lake of the Ozarks at Niangua Arm Largemouth Bass Fish muscle plug 0.15 0.030 55904 2011-025-406-2 Lake of the Ozarks at Niangua Arm Largemouth Bass Fish muscle plug 0.28 0.055 55905 2011-025-406-3 Lake of the Ozarks at Niangua Arm Largemouth Bass Fish muscle plug 0.46 0.093 55906 2011-025-406-4 Lake of the Ozarks at Niangua Arm Largemouth Bass Fish muscle plug 0.46 0.092 55907 2011-025-406-5 Lake of the Ozarks at Niangua Arm Largemouth Bass Fish muscle plug 0.30 0.060

55908 2011-025-406-6 Lake of the Ozarks at Niangua Arm Largemouth Bass Fish muscle plug 0.28 0.05655909 2011-679-406-1 Longview Lake Largemouth Bass Fish muscle plug 1.13 0.23

55910 2011-679-406-2 Longview Lake Largemouth Bass Fish muscle plug 0.80 0.16
Results 

9

Table 4. Concentrations of total mercury in fish fillets, fish muscle plugs, and crayfish tissues.—Continued[USGS, U.S. Geological Survey; MDC, Missouri Department of Conservation; Hg, mercury; μg/g, micrograms per gram; wet weight concentrations estimated assuming 80 percent moisture].

 USGS

ID

MDC

ID Site location Biota common name Matrix Hg μg/g dry weight Hg μg/g wet weight

55911 2011-679-406-3 Longview Lake Largemouth Bass Fish muscle plug 0.89 0.18

55912 2011-679-406-4 Longview Lake Largemouth Bass Fish muscle plug 1.50 0.30

55913 2011-679-406-5 Longview Lake Largemouth Bass Fish muscle plug 0.98 0.20

55914 2011-679-406-6 Longview Lake Largemouth Bass Fish muscle plug 0.98 0.20

55915 2011-118-406-1 Stockton Lake at Big Sac Arm Largemouth Bass Fish muscle plug 0.19 0.038

55916 2011-118-406-2 Stockton Lake at Big Sac Arm Largemouth Bass Fish muscle plug 0.26 0.053

55917 2011-118-406-3 Stockton Lake at Big Sac Arm Largemouth Bass Fish muscle plug 0.43 0.086

55918 2011-118-406-4 Stockton Lake at Big Sac Arm Largemouth Bass Fish muscle plug 0.28 0.057

55919 2011-118-406-5 Stockton Lake at Big Sac Arm Largemouth Bass Fish muscle plug 0.13 0.027

55920 2011-118-406-6 Stockton Lake at Big Sac Arm Largemouth Bass Fish muscle plug 0.49 0.10

55921 2011-165-406-1 Clearwater Lake Largemouth Bass Fish muscle plug 2.84 0.57

55922 2011-165-406-2 Clearwater Lake Largemouth Bass Fish muscle plug 4.74 0.95

55923 2011-165-406-3 Clearwater Lake Largemouth Bass Fish muscle plug 2.48 0.50

55924 2011-165-406-4 Clearwater Lake Largemouth Bass Fish muscle plug 2.88 0.58

55925 2011-165-406-5 Clearwater Lake Largemouth Bass Fish muscle plug 1.76 0.35

55926 2011-165-406-6 Clearwater Lake Largemouth Bass Fish muscle plug 1.89 0.38

55927 2011-241-406-1 Lake St. Louis Largemouth Bass Fish muscle plug 1.83 0.37

55928 2011-241-406-2 Lake St. Louis Largemouth Bass Fish muscle plug 1.01 0.2055929 2011-241-406-3 Lake St. Louis Largemouth Bass Fish muscle plug 0.75 0.1555930 2011-241-406-4 Lake St. Louis Largemouth Bass Fish muscle plug 0.70 0.1455931 2011-241-406-5 Lake St. Louis Largemouth Bass Fish muscle plug 0.44 0.08855932 2011-241-406-6 Lake St. Louis Largemouth Bass Fish muscle plug 1.44 0.2955933 2011-345-406-1 Noblett Lake Largemouth Bass Fish muscle plug 1.75 0.35

55934 2011-345-406-2 Noblett Lake Largemouth Bass Fish muscle plug 1.45 0.29

55935 2011-345-406-3 Noblett Lake Largemouth Bass Fish muscle plug 1.27 0.25

55936 2011-345-406-4 Noblett Lake Largemouth Bass Fish muscle plug 1.90 0.38

55937 2011-345-406-5 Noblett Lake Largemouth Bass Fish muscle plug 2.22 0.44

55938 2011-345-406-6 Noblett Lake Largemouth Bass Fish muscle plug 0.97 0.19

55939 2011-704-406-1 Hazel Creek Lake Largemouth Bass Fish muscle plug 1.76 0.35

55940 2011-704-406-2 Hazel Creek Lake Largemouth Bass Fish muscle plug 2.12 0.42

55941 2011-704-406-3 Hazel Creek Lake Largemouth Bass Fish muscle plug 1.85 0.37

55942 2011-704-406-4 Hazel Creek Lake Largemouth Bass Fish muscle plug 0.87 0.17

55943 2011-704-406-5 Hazel Creek Lake Largemouth Bass Fish muscle plug 2.03 0.41
10 Concentrations of Elements in Fish Fillets, Fish Muscle Plugs, and Crayfish from the 2011 Contaminant Monitoring Program Table 4. Concentrations of total mercury in fish fillets, fish muscle plugs, and crayfish tissues.—Continued [USGS, U.S. Geological Survey; MDC, Missouri Department of Conservation; Hg, mercury; μg/g, micrograms per gram; wet weight concentrations estimated assuming 80 percent moisture]. USGS ID MDC ID Site location Biota common name Matrix Hg μg/g dry weight Hg μg/g wet weight 55944 2011-704-406-6 Hazel Creek Lake Largemouth Bass Fish muscle plug 3.57 0.71 55945 2011-713-406-1 Harrison County Lake Largemouth Bass Fish muscle plug 1.49 0.30 55946 2011-713-406-2 Harrison County Lake Largemouth Bass Fish muscle plug 1.74 0.35 55947 2011-713-406-3 Harrison County Lake Largemouth Bass Fish muscle plug 1.47 0.29 55948 2011-713-406-4 Harrison County Lake Largemouth Bass Fish muscle plug 1.98 0.40 55949 2011-713-406-5 Harrison County Lake Largemouth Bass Fish muscle plug 3.34 0.67 55950 2011-713-406-6 Harrison County Lake Largemouth Bass Fish muscle plug 1.73 0.35 55952 2011-134-609-1-S Big River at Cherokee Landing Crayfish species Carcassa 0.028 0.006 55954 2011-134-609-2-S Big River at Cherokee Landing Crayfish species Carcass 0.037 0.007 55956 2011-134-609-3-S Big River at Cherokee Landing Crayfish species Carcass 0.017 0.003 55958 2011-134-609-4-S Big River at Cherokee Landing Crayfish species Carcass 0.026 0.005 55960 2011-134-609-5-S Big River at Cherokee Landing Crayfish species Carcass 0.029 0.006 55962 2011-134-609-6-S Big River at Cherokee Landing Crayfish species Carcass 0.024 0.005 55964 2011-134-609-7-S Big River at Cherokee Landing Crayfish species Carcass 0.029 0.006 56227a 2011-134-609-M Compositeb Big River at Cherokee Landing Crayfish species Tail meat 0.052 0.010 55965 2011-726-609-1-M Shoal Creek 0.5 mile North of I-44 Bridge Crayfish species Tail meat 0.023 0.005 55966 2011-726-609-1-S Shoal Creek 0.5 mile North of I-44 Bridge Crayfish species Carcass 0.008 0.002 55967 2011-726-609-2-M Shoal Creek 0.5 mile North of I-44 Bridge Crayfish species Tail meat 0.019 0.004 55968 2011-726-609-2-S Shoal Creek 0.5 mile North of I-44 Bridge Crayfish species Carcass 0.010 0.002 55969 2011-726-609-3-M Shoal Creek 0.5 mile North of I-44 Bridge Crayfish species Tail meat 0.027 0.005 55970 2011-726-609-3-S Shoal Creek 0.5 mile North of I-44 Bridge Crayfish species Carcass 0.011 0.002 55971 2011-726-609-4-M Shoal Creek 0.5 mile North of I-44 Bridge Crayfish species Tail meat 0.022 0.004 55972 2011-726-609-4-S Shoal Creek 0.5 mile North of I-44 Bridge Crayfish species Carcass 0.008 0.002 55973 2011-726-609-5-M Shoal Creek 0.5 mile North of I-44 Bridge Crayfish species Tail meat 0.029 0.006 55974 2011-726-609-5-S Shoal Creek 0.5 mile North of I-44 Bridge Crayfish species Carcass 0.013 0.003 55975 2011-726-609-6-M Shoal Creek 0.5 mile North of I-44 Bridge Crayfish species Tail meat 0.011 0.002 55976 2011-726-609-6-S Shoal Creek 0.5 mile North of I-44 Bridge Crayfish species Carcass 0.008 0.002 55977 2011-726-609-7-M Shoal Creek 0.5 mile North of I-44 Bridge Crayfish species Tail meat 0.012 0.002 55978 2011-726-609-7-S Shoal Creek 0.5 mile North of I-44 Bridge Crayfish species Carcass 0.006 0.001 55979 2011-726-609-8-M Shoal Creek 0.5 mile North of I-44 Bridge Crayfish species Tail meat 0.011 0.002

55980 2011-726-609-8-S Shoal Creek 0.5 mile North of I-44 Bridge Crayfish species Carcass 0.012 0.00255981 2011-726-609-8-T Shoal Creek 0.5 mile North of I-44 Bridge Crayfish species Tail shell <0.005 <0.001

55982 2011-726-609-9-M Shoal Creek 0.5 mile North of I-44 Bridge Crayfish species Tail meat 0.008 0.002
 Quality-Control Results 11

Table 4. Concentrations of total mercury in fish fillets, fish muscle plugs, and crayfish tissues.—Continued[USGS, U.S. Geological Survey; MDC, Missouri Department of Conservation; Hg, mercury; μg/g, micrograms per gram; wet weight concentrations estimated assuming 80 percent moisture].

 USGS

ID

MDC

ID Site location Biota common name Matrix Hg μg/g dry weight Hg μg/g wet weight

55983 2011-726-609-9-S Shoal Creek 0.5 mile North of I-44 Bridge Crayfish species Carcass 0.012 0.002

55984 2011-726-609-9-T Shoal Creek 0.5 mile North of I-44 Bridge Crayfish species Tail shell <0.005 <0.001

55985 2011-726-609-10-M Shoal Creek 0.5 mile North of I-44 Bridge Crayfish species Tail meat 0.007 0.00155986 2011-726-609-10-S Shoal Creek 0.5 mile North of I-44 Bridge Crayfish species Carcass 0.010 0.002

55987 2011-726-609-10-T Shoal Creek 0.5 mile North of I-44 Bridge Crayfish species Tail shell <0.005 <0.001

aCarcass is defined as crayfish remains after tail meat has been removed or extracted.bBecause of insufficient biomass in submitted individual samples, this sample is a composite of seven crayfish tail meat samples collected from the Big River at Cherokee Landing (55951, 

55953, 55955, 55957, 55959, 55961, 55963).

levels were markedly higher in crayfish carcass samples 

from the Big River at Cherokee Landing (3 to 7.8 μg/g dry 

weight; USGS IDs 55952-55964) and tail-meat levels were 

most elevated in the tail meat composite sample from this site 

(1.06 μg/g dry weight; USGS ID 56227). Cadmium concentra-

tions (μg/g dry weight) in crayfish tissues collected from the 

one remaining site (Shoal Creek; USGS IDs 55965-55987) 

ranged as follows: carcass, 0.2 to 0.5; tail shell, 0.02 to 0.042; 

and tail meat, 0.017 to 0.33. Lead concentrations (μg/g 

dry weight) in fish fillet samples mostly were less than 0.5 

(76 percent of the sample set), whereas remaining samples 

ranged from 0.81 to 1.5. All crayfish tissues from Shoal Creek 

exhibited Pb concentrations ranging from 0.17 to 4.74 μg/g 

dry weight. This is in sharp contrast to Pb concentrations in 

crayfish carcass samples and a tail meat composite in cray-

fish collected from Cherokee Landing (21.9 to 44.9 μg/g dry 

weight). 

All fish fillet samples exhibited Hg concentrations 

less than the current (2009) U. S. Environmental Protection 

Agency (USEPA) Water Quality Criterion for Hg of 0.30 μg/g 

wet weight (table 4), or about 1.5 μg/g dry weight based on an 

80 percent moisture content (U. S. Environmental Protection 

Agency, 2001); however, a number of dorsal fish muscle plugs 

collected from largemouth bass exceeded this criterion, and 

the site, number of plugs, and Hg concentration ranges (μg/g 

dry weight) were as follows: Clearwater Lake, 6 plugs, 1.76 to 

4.74; Lake St. Louis, 1 plug, 1.83; Noblett Lake, 3 plugs, 1.75 

to 2.22; Hazel Creek Lake, 5 plugs, 1.76 to 3.57; Harrison 

County Lake, 4 plugs, 1.73 to 3.34. Mercury concentrations 

in all crayfish tissues were quite low (less than 0.06 μg/g dry 

weight). 

 Quality-Control Results

Calibration Verification.—A calibration blank and an 

independent calibration verification standard (ICVS) were 

analyzed every 10 samples to confirm the calibration status 

of the ICP-MS during instrumental analyses of the fish fillets, 

fish muscle plugs, and crayfish tissues for Ca, Zn, Cd, and Pb; 

blanks were within plus or minus (±)three times the instrument 

detection limits for each element, and ICVS recoveries were 

within the target of 90 to 110 percent of the ICVS standard 

concentration for each element. Three reference solutions 

[National Institute of Standards and Technology (NIST) 

Standard Reference Material (SRM) 1640a: Trace Elements in 

Natural Water; Spex ClaritasPPT Instrument Check Standard 

1 (Spex ICS-1); and High Purity Standards Certified Refer-

ence Solution Trace Metals in Fish: HP CRM-TF] used as 

laboratory-control samples exhibited elemental recoveries 

ranging from 98 to 100 percent. Calibration verification refer-

ence tissues for total Hg [National Research Council Canada 

(NRCC) DOLT-3: Dogfish Liver; International Atomic Energy 

Agency (IAEA) 407-Trace Elements and Methylmercury 

in Fish Tissue] were analyzed at the beginning and end of 
12 Concentrations of Elements in Fish Fillets, Fish Muscle Plugs, and Crayfish from the 2011 Contaminant Monitoring Program

the instrumental runs to confirm the calibration status of the 

DMA-80 system; percent errors were within the target of ±10 

percent. 

Reference Materials.—Recoveries of Ca, Zn, Cd and Pb 

in three tissue reference materials (NIST 1566a: Oyster Tissue, n=1; IAEA 407: Whole-body Fish, n=1; NRCC TORT-1: 

Lobster Hepatopancreas, n=1) ranged from 80 to 120 percent 

and averaged 100 percent. Recoveries of Hg from six different tissue reference materials (IAEA MA-A-1: Copepod, n=4; 

IAEA MA-A-2: Fish Flesh Homogenate, n=4; IAEA 407: 

Whole-body Fish, n=4; NIST RM50: Albacore Tuna, n=1; 

NRCC DOLT-3: Dogfish Liver, n=4; and NRCC DORM-2: 

Dogfish Fillet, n=4;) ranged from 89 to 105 percent and averaged 98 percent.

Method and Instrumental Precision.— Method precision as estimated from measurement variation for triplicate 

digestion and analysis of a fish fillet sample had percent 

relative standard deviations (PRSDs) for Ca, Zn, and Cd that 

were less than or equal to (≤) 26, but 60 for Pb; however, the 

higher variation for Pb was not considered unusual because 

two of the three sample concentrations were below the method 

quantitation limit of 0.026 μg/g dry weight. PRSDs for the 

elements from a crayfish carcass replicate were ≤ 10. Relative percent differences (RPDs) from the duplicate digestion 

and analysis of the crayfish tail meat composite sample were 

≤ 21 for Ca, Zn, and Pb, but higher (40) for Cd. All PRSDs for 

Hg (n=4) were less than (<) 9 percent. Instrumental precision 

measured as RPD from the analysis of fish fillet (n= 3) and 

crayfish tail meat (n=3) duplicate digestates for Ca, Zn, Cd, 

and Pb was < 5 percent. 

Spikes.— Recoveries of Zn, Cd, and Pb spiked into fish 

tissue (n=2) ranged from 105 to 107 percent and averaged 

106 percent, whereas Ca spike recoveries were 111 and 145 

percent. Recoveries of all four elements in spiked crayfish tissues (n=2) ranged from 103 to 120 percent and averaged 111 

percent. Recoveries of methylmercury hydroxide spiked into 

fish fillet (n=2), fish muscle plugs (n=4), and crayfish tissue 

(n=2) ranged from 70 to 101 percent and averaged 88 percent. 

Post-digestion or analysis spikes for Ca, Zn, Cd, and Pb in fish 

fillets (n=3) and crayfish tissues had recoveries ranging from 

81 to 105 percent and averaged 96 percent. 

Interference Checks.— As a check for potential interferences, dilution percent differences (DPDs) based on fivefold 

dilutions of fish fillet (n=3) and crayfish tail-meat digestates 

were determined. DPDs were ≤ 11 percent for Zn, Cd, and Pb, 

but higher for Ca (14 to 27 percent), suggesting some suppression of the Ca signal in these matrices. A synthetic solution 

containing high concentrations of aluminum, Ca, iron, magnesium, sodium, phosphorus, potassium, sulfur, carbon, molybdenum, and titanium was analyzed (n=4) to observe the effects 

of these potential interfering elements on the determination of 

Zn, Cd, and Pb concentrations in this matrix. Recoveries were 

within the 80 to 120 percent tolerance

Blank Equivalent Concentrations (BEC).— BECs (μg/g 

dry weight, Ca, Zn, Cd, Pb) for digestion blanks prepared 

with each batch were determined; all BECs were less than the 

corresponding method detection limits (MDLs) except for one 

instance of Zn (0.16 BEC compared to 0.11 μg/g MDL), one 

instance of Cd (0.002 BEC compared to 0.002 μg/g MDL), 

and one instance of Pb (0.009 BEC compared to 0.007μg/g 

MDL). The BEC exceptions each represent low concentrations 

that were not considered unusual. All BECs for Hg were less 

than the corresponding Hg MDLs 

Instrument Detection, Method Detection, and Method 

Quantitation Limits.—The instrument detection limit (IDL) 

for Hg was 0.002 nanograms (ng); the IDLs for other target 

analytes in nanograms per milliliter were as follows: Ca, 2.3; 

Zn, 0.9; Cd, 0.003; and Pb, 0.004. MDLs were computed in 

μg/g dry weight for each batch of samples as:

3 X (SDb

2

 + SDs

2

)1/2

where 

SDb = standard deviation of a blank (n=3); and 

SDs = standard deviation of a low level sample or 

spiked sample (n=3) 

and were as follows:Ca, 1.6 to 2.9; Zn, 0.03 to 0.6; Cd, 0.002 

to 0.012; Hg, 0.005 to 0.042; and Pb, 0.007 to 0.009. Method 

quantitation limits (MQLs) were calculated in μg/g dry weight 

as 3.3 x MDLs and were as follows: Ca, 5.3 to 9.6; Zn, 0.1 to 

2.0; Cd, 0.007 to 0.040; Hg, 0.018 to 0.14; and Pb, 0.023 to 

0.030.

All quality-control results for the study were within 

acceptable limits as specified by USGS.

References Cited

Schmitt, C.J., and Finger, S.E., 1987, The effects of sample 

preparation on measured concentrations of eight elements 

in edible tissues of fish from streams contaminated by lead 

mining: Archives of Environmental Contamination and 

Toxicology, v.16, p.185-207.

U. S. Environmental Protection Agency, 1998, Mercury in 

solids and solutions by thermal decomposition, amalgamation, and atomic absorption spectrophotometry: accessed 

August 28, 2007, at http://www.epa.gov/epaoswer/hazwaste/

test/up4a.htm#7_series.

United States Environmental Protection Agency, 2001, Water 

quality criterion for protection of human health - Methylmercury: Washington D.C., U. S. Environmental Protection 

Agency, Office of Water, EPA-823-R-01-001, 16 p.
Publishing support provided by: 

Rolla Publishing Service Center 

For more information concerning this publication, contact:

Director, USGS Columbia Environmental Research Center

4200 New Haven Road

Columbia, MO 65201

(573) 875–5399

Or visit the Columbia Environmental Research Center Web site at:

http://www.cerc.usgs.gov/
May and others—Concentrations of Elements in Fish Fillets, Fish Muscle Plugs, and Crayfish from the 2011 Contaminant Monitoring Program—OFR 2012–1268