bluuebunny/crossref_metadata_2025_split huggingface dataset:
Analytical Procedures Used in FDA Laboratories for the
Analysis of Hallucinogenic Drugs
Authors: Martin Robert J , Alexander Thomas G 
Published: February 2020

Abstract
Various ultraviolet, infrared, and TLC procedures are described for the separation and identification of hallucinogenic drugs. Specific methods for LSD, DMT, and psilocybin are also presented, along with general background information for the hallucinogenic drugs.
Partition Chromatographic Assay of Opium and
Opium Preparations
Authors: Smith Edward , Levine Joseph , Banes Daniel 
Published: February 2020

Abstract
Application of column partition chromatography to opium extracts provides quantitative recovery of spectrophotometrically pure morphine. The extract is prepared by homogenizing opium with water in a highspeed blender or by evaporating paregoric to remove alcohol. An entire assay can be performed within 3 hours.
Extraction and Cleanup Procedure for the Gas
Chromatographic Determination of Four Dinitrophenolic Pesticides
Authors: Yip George , Howard Samuel F 
Published: February 2020

Abstract
A gas chromatographic method for the simultaneous determination of four dinitrophenolic herbicides [dinitrocresol (DNOC), dinitrobutylphenol (DNBP), dinitroamylphenol (DNAP), and dinitrocyclohexylphenol (DNOCHP)] in crops has been developed. After a 50 g sample was extracted with chloroform, a 10 g aliquot was concentrated and reacted with diazomethane to form the methyl ether derivatives. The sample was subjected to a two column cleanup step. acid-Celite and Florisil, and the residue was analyzed by GLC with an electron capture detector. Recoveries of fortification levels of 0.1 ppm DNOC and 0.2 ppm DNBP, DNAP, and DNOCHP exceeded 80%. The crops studied included green beans, pole beans, lima beans, peas, apples, and oranges.
Screening Method for Zearalenone., Aflatoxin, and
Ochratoxin
Authors: Eppley R M 
Published: February 2020

Abstract
A rapid and sensitive procedure has been developed for detecting aflatoxin, ochratoxin, and zearalenone. This procedure uses a water-chloroform extraction combined with sequential elution of the mycotoxins from a silica gel column. Applicability to a wide variety of products was demonstrated by analysis of 31 different commodities. Three commodities (cottonseed, green coffee, and capsicum peppers) contained serious interferences for all three toxins.
Preparation of Dehydrated Tomato Powder Samples for
Howard Mold Count
Authors: Krinitz Benjamin 
Published: February 2020

Abstract
Collaborative studies were conducted on two procedures for preparing dehydrated tomato products for analysis by the Howard mold count method, 36.069: Procedure I, a modification of method 36.069, which involves a simple dilution and the determination of per cent solids by refractive index; and Procedure II (FDA procedure), which involves heating and weighing after the calculation of the dilution necessary to give the desired per cent solids. Results indicate that Procedure I is a simple and rapid means of preparing dehydrated tomato powder.
A New Extraction Method for Light Filth in Ground and Granulated Pecans
Authors: Vazquez Alberto Wanous , Gecan John S 
Published: February 2020

Abstract
A method has been developed that gives good filth recoveries and clean, easy to scan, filter papers. This method deviates from method 36.018 by using 60% alcohol-calcium chloride solution for the aqueous phase and light mineral oil as the flotation medium. Acid hydrolysis in the trap flask, together with the low viscosity and desirable surface properties of alcohol, aids in suppressing plant material. The added calcium chloride gives a high enough density to the aqueous phase to permit denser filth elements to float with ease.
Collaborative Study of the Determination of Ethoxyquin in Chick Tissue and Eggs by Fluorescence
Authors: Deren J M Van , Jaworski E G 
Published: February 2020

Abstract
A collaborative study for the analysis of ethoxyquin was repeated with a modified procedure for the preparation of the standard curve, and all standard curves were satisfactory. Ethoxyquin recovery was good in all tissues analyzed: 76% from egg yolks (lowest recovery) and 88% from fat (highest recovery). The fluorescent spectrum for ethoxyquin shows that the secondary filter is quite critical; light scattering from the sample must be controlled to avoid interferences. Although variation in the control samples was caused by both the source of the tissue samples and the secondary filters, values did not exceed the 10% tolerance level established for ethoxyquin in tissue and eggs. It is recommended that this modified method be adopted as official, first action.
Collaborative Study of a Method for Benzo(a)pyrene in Smoked Foods
Authors: Howard John W , Fazio Thomas , White Richard H 
Published: February 2020

Abstract
A collaborative study was conducted on the method for benzo(a)pyrene in smoked foods published in This Journal 49, 611-617 (1966). Samples of fish and ham fortified with benzo(a)pyrene were analyzed by 13 collaborators. Average per cent recoveries at 10 and 4 ppb (μg/kg) levels by 11 collaborators by the ultraviolet method were 99 and 96%, respectively, for the fortified fish samples and 84 and 78%, respectively, for the fortified ham samples. Comparative average recovery values were obtained by 6 collaborators who also determined the compound by fluorescence. Standard deviations for the two determinative techniques ranged from 3.15 to 13.6%. The method is recommended for adoption as official, first action.
Rapid Analysis of Halogenated Organic Insecticides in Aqueous Animal Dips, Using Sodium Biphenyl
Authors: Czech Fred P 
Published: February 2020

Abstract
Pertinent parameters for an analytical method, using sodium biphenyl, are presented for the quantitative estimation of toxaphene, lindane, DDT, methoxychlor, dieldrin, chlordane, ronnel, Ruelene, eoumaphos, trichlorfon, and naled in aqueous dips. The method is applicable to both insecticide emulsion and wettable powder dips.
Differential Spectrometric Determination of Caffeine in Soluble Coffee and in Drug Combinations
Authors: Ferren William P , Shane Norman A 
Published: February 2020

Abstract
A differential spectrophotometric procedure is described for determining caffeine in food and beverage materials and in drug dosage combinations. The method eliminates the necessity for preliminary separations. The procedure was applied to soluble coffee samples and to APC. Recovery of caffeine from soluble coffee was better than 95% ; results compared favorably with the official micro Bailey-Andrew method. Results for APC were not as good; apparently phenacetin is the limiting factor. The method may be more suitable for other drug combinations or for certain types of automated analyses.
Collaborative Study of a Method and Sampling Techniques For Determining Yeast Count in Maple Sirup
Authors: Kissinger J C 
Published: February 2020

Abstract
Techniques for sampling and a method for determining the yeast count in maple sirup, studied collaboratively in 1966, have been revised and again studied collaboratively in 18 laboratories. Statistical analysis of collaborators' results indicated that sirup samples shipped in a frozen condition gave more concordant interlaboratory yeast counts. More homogeneous cell suspensions were obtained by mixing the sirup samples warmed to 80 °F with a nonaerating stirrer. The method is recommended for adoption as official, first action.
Quantitative Analysis of Phenaglycodol
Authors: Snell Robert P 
Published: February 2020

Abstract
A procedure has been developed for the quantitative and qualitative infrared spectrophotometric analysis of phenaglycodol in tablets and capsules. The procedure consists of a liquid-liquid partition of the drug between chloroform and an aqueous alkaline phase. The quantitative measurement is made at about 9.85 μ relative to a carbon disulfide reference, using the baseline technique. Qualitative analysis employs the KBr disk technique. Five collaborators obtained a relative standard deviation of ± 1.88% for a tablet preparation and ± 1.61% for a capsule preparation. It is recommended that the method be adopted as official, first action.
Collaborative Study of a Spiral Vessel Count Method for Estimating Shell in the Chocolate Component of Cocoa and Related Products
Authors: Jackson Manion M 
Published: February 2020

Abstract
Part-I: The spiral vessel count method for estimating pectic acid in cocoa has been modified to replace the saturated borax solution by 4% NaOH, which gives a clearer product to count, and to include a method for preparing the sample dry fat-free and 250 mesh before analyzing, by hand grinding or grinding by two different grinders. Counts have been made on known shell in the chocolate component mixtures. A formula usable in a 1—15% range and standard curves have been prepared for the estimation of shell in the chocolate component. Counts have been taken at 100X and 200x on a 0.2 g/100 ml concentration, and at 200X on a 0.35 g/50 ml concentration; 200X counting of the higher concentration is preferred for 1—15% shell. Cocoas of known pectic acid content were analyzed by the method and per cent shell found by spiral vessel counts compared with per cent pectic acid. These cocoas were also analyzed before being made 250 mesh for comparative purposes. An intralaboratory study was made on two samples. Part-II: A collaborative study for determining per cent shell by the spiral vessel count method was made on four samples of cocoa products by six collaborators; two samples were defatted and ground to 250 mesh, the other two samples were hand-ground. Five collaborators varied less than 1 standard deviation unit from the average on the four subdivisions; one collaborator was just outside the standard deviation on one sample. The precision of the results was within a reasonable range for a microscopic counting procedure, and the method has been recommended for adoption as official, first action.
Determination of Lignin and Cellulose in Acid-Detergent Fiber with Permanganate
Authors: Van Soest P J , Wine R H 
Published: February 2020

Abstract
A newly developed indirect method for lignin, utilizing permanganate, permits the determination of cellulose and insoluble ash in the same sample. The new permanganate lignin method is intended as an alternative procedure to the 72% sulfuric acid method over which it offers definite advantages as well as certain disadvantages. Choice of methods will depend upon the materials analyzed and the purpose for which the values are to be used.
EDTA Titration of Calcium and Magnesium: Determination of Calcium in Canned Vegetables
Authors: Steagall Edward F 
Published: February 2020

Abstract
The method adopted as official, final action last year was studied collaboratively again this year for calcium in canned vegetable products other than canned whole tomatoes. Twenty-six cans each of whole potatoes with calcium declared on the label and sliced potatoes and lima beans without a label declaration for calcium were analyzed by 13 analysts in 12 laboratories. Again the results were easily reproducible, and the agreement between laboratories was good. Because the method gives continuing precision and low standard deviations, it is recommended for adoption as official, final action for pharmaceutical and vitamin-mineral preparations and canned whole tomatoes, and as official, first action for canned potatoes and lima beans.
Collaborative Study of a New Alkaline Phosphatase Assay System for Milk
Authors: Kleyn D H , Lin S H C 
Published: February 2020

Abstract
A new method in which phenolphthalein monophosphate is used as substrate has been developed for determining residual alkaline phosphatase: Upon hydrolysis, phenolphthalein is released and yields a red solution that is compared visually with a standard prepared from the same milk. Seven collaborators made 168 observations that were used in a statistical study of the results. Chi-square calculations and tests of independence indicated that the described method yields results on skim milk, whole milk, and light cream that are as precise and either as accurate or more accurate than those obtained with the Scharer I method. Based on these results, it is recommended that the method be adopted as official, first action.
Collaborative Study of the Determination of Lead Number of Vanilla Extract By Chelometric Titration
Authors: Johnson Arthur R 
Published: February 2020

Abstract
The Wichmann lead number has been used for over 45 years as an index of vanilla constituents in extracts. A rapid method for lead number determination by chelometric titration was reported by Considine in 1959. This method was subjected to intralaboratory and collaborative study. On the basis of these results, the method is rapid and accurate, and it is recommended for adoption as official, first action.
Review and Recommended Changes in the Flame Photometric Method for Determination of Potassium in Fertilizers
Authors: Hambleton Larry G 
Published: February 2020

Abstract
Ammonium oxalate is, historically, the oldest extractant for available potassium in fertilizer. Lower results have been obtained by the flame photometric method, 2.077, than with the other official methods, possibly because of the extractant, ammonium carbonate. It is recommended that the preparation of solution 2.079(a) be changed to indicate ammonium oxalate as the extractant in place of ammonium carbonate.
Isolation and Purification of Metabolites Found in the Urine of Male Rats Fed Aldrin and Dieldrin
Authors: Klein A K , Link J D , Ives N F 
Published: February 2020

Abstract
A procedure for the isolation and purification of aldrin and dieldrin metabolites derived from rat urine is described. The procedure yields enough material of adequate purity to enable the determination of the chemical structure of the metabolites.
Collaborative Study of Recoverable Oil in Citrus Juices by Bromate Titration
Authors: Scott W Clifford 
Published: February 2020

Abstract
Nineteen collaborators conducted single tests on three citrus juices containing abovit 0.005, 0.010, and 0.030% oil. Standard deviations in per cent recoverable oil were 0.0004, 0.0008, and 0.0014, respectively. Each collaborator also titrated in triplicate a 0.035% solution of freshly distilled orange oil in 2-propanol. The average amount found was 0.0345%, with a standard deviation of 0.0007. The method is recommended for adoption as official, first action.
Isothermal Molecular Weight Determination: Apparatus, Procedure, and Study of Effect of Solvent and Standard on Accuracy and Precision
Authors: Scroggins Laverne H , Ogg C L 
Published: February 2020

Abstract
A study was made of the isothermal molecular weight determination; the apparatus constructed and the procedure developed are described. An extensive investigation was carried out to provide reliable guides for the selection of the correct solvents and standard reference compounds to be used in the molecular weight determination. This study produced statistical evidence of the behavior, in five different solvents, of representative compounds from each of the following chemical groups: hydrocarbons, alcohols, ketones, esters, ethers, acids, nitriles, amines, and sulfides. Analysis showed that acetone and ethyl acetate are the best solvents if the composition of the sample is not known. Chloroform proved to be a good solvent except for samples in which hydrogen bonding could occur. n-Heptane was satisfactory for six of the eight types of compounds; benzene war. by far the poorest solvent
Correlation of the Levels of Several Constituents of Commercial Orange Juices
Authors: Coffin D E 
Published: February 2020

Abstract
The amino acid, betaine, polyphenolics, ash, and phosphorus contents, and the titratable acidity of 32 samples of commercial orange juices and reconstituted orange juices were determined. Wide variations in the levels of these constituents were found but there were no significant differences between the juices and the reconstituted juices. Highly significant correlations were established between the levels of the amino acids, betaine, polyphenolics, ash, and phosphorus. The titratable acidity levels failed to show any significant correlation to any of the other constituents. Multiple regression equations were developed to express the interrelationships between some of the components, and correlation coefficients of combined distributions were calculated.
Determination of Organic Acids in Vanilla Extracts by GLC Separation of Tnmethylsilylated Derivatives
Authors: Fitelson J , Bowden George L 
Published: February 2020

Abstract
A method for the analysis of organic acids in vanilla extracts has been developed. The lead salts of the organic acids are separated, trimethylsilylated derivatives are formed directly from the lead salts, and the trimethylsilylated de rivatives are separated by GLC. Typical vanilla chromatograms show about 20 acid peaks, with 8 major ones. The main vanilla acid shows up as the largest peak, identified as 7. Malic acid occurs naturally in vanilla and is measured by Peak 2. Tahiti extracts are distinguished from other extracts by the smaller Peak 2, and the ratio of Peak 7 to Peak 2 can be used to identify these extracts. To measure the peak heights on a standard basis, known quantities of glutaric acid are added to the vanilla extract sample; this internal standard appears between vanilla acid Peaks 1 and 2. Gross deficiency in vanilla solids in the extract is detected by low peak heights; additions of foreign acids are readily shown by abnormal peak heights or by foreign peaks. This method was studied by ten collaborators and the unknowns were identified correctly. The proposed method provides more information in a shorter time than any method or combination of methods now available. However, since each GLC instrument has different responses to the same set of empirical conditions given in the method, each analyst must test authentic extracts and establish the characteristics to be used for the basis of comparison. The method is recommended for adoption as official, first action.
Collaborative Study of a Colorimetric Method for Paraquat in Formulations
Authors: Carlstrom A A 
Published: February 2020

Abstract
A colorimetric method described by Yuen, Bagness, and Myles in 1967 was collaboratively studied with paraquat formulations containing 2 lb/gal. (about 20% cation). Paraquat is determined in a diluted solution by measuring the absorbance, at 600 mμ, of the blue free radical produced by reduction with alkaline sodium dithionite, and its absorbance is compared to a reference standard curve. Standard deviation estimation of random error was 0.22 for paraquat dimethylsulfate formulations and 0.26 for paraquat dichloride. Standard deviation estimates of systematic error were 0.20 and 0.62, respectively. The method is recommended for adoption as official, first action.
Colorimetric Determination of Ronidazole in Feeds
Authors: Szalkowski C R , Kanora J 
Published: February 2020

Abstract
Ronidazole, (l-melhyl-5-nitroimidazoI- 2-yl)mcthyl carbamate, is extracted from finished poultry feeds with methanol and chromatographcd on an AL2O3-FIorex column. The eluate is concentrated and dissolved in CCI4 and the ronidazole is extracted with. H2O. The purified ronidazole is hydrolyzcd in NaOH solution in the presence of copper and p-aminobenzoic acid; the resulting diazonium compound is then coupled with naphthylethylenediamine to form a colored complex, which is measured spectrophotometrically at 550 mµ. No significant interference was found from finished feeds, domestic and foreign, or from 48 common feed additives. Recovery experiments on 36 laboratory-prepared feed samples at levels ranging from 0.0015 to 0.030% ronidazole averaged 100.8% with a standard deviation of 2.4.
Thin Layer Densitometric Determination of Rotenone and Deguelin
Authors: Delfel Norman E , Tallent William H 
Published: February 2020

Abstract
Rutenone and deguelin are separated by chromatography on silver nitrate-impregnated silica gel G with chloroform acetone: acetic acid (196:3:1) solvent system. Glass plates, 20 × 20 cm, are coated with a special spreader producing a 0.25 mm layer and a 1.00 mm band at the upper end. Since additional solvent is required to saturate the thicker band, such plates give resolutions comparable to plates twice as long. Developed plates are treated with nitric acid vapor, then ammonia vapor, to produce dark spots for the rotenoids. Plates are scanned with a commercial densitometer, and the quantity of rotenoids is calculated from peak area in the resultant curve. Kecoveries of rotenone and deguelin added to extracts of Tephrosia vogelii, Lonchocarpus nicou, and Derris elliptica averaged 104.1 and 99.4%, respectively. The standard deviation of the method applied to plant extracts was 7.9% for rotenone and 8.3% for deguelin. The amounts of rotenone in the L. nicou samples were comparable to those determined by the AOAC crystallization and infrared methods.
A New Approach to the Raney Catalyst Powder Method for Total Nitrogen in Fertilizers
Authors: Brabson J A , Woodis T C 
Published: February 2020

Abstract
Further study of the Raney catalyst powder method for the determination of nitrogen in fertilizers established conditions in which the commercial alloy containing 50% Ni and 50% Al was a more efficient reductant for nitrates than an experimental alloy that contained 10% Co. Errors in measurement were decreased, accuracy was increased, and time was saved by adding all the sulfuric acid and part of the potassium sulfate as a single dilute solution and heating the mixture immediately to promote the reduction. Changes in the amounts of reagents, including use of the contents of a Kcl-Pak without the polyethylene envelope, resulted in smoother and more effective Kjeldahl digestions. The method is “rugged” and is equally applicable to the refractory compound nicotinic acid, mixtures of nitrates and organic materials, and the simplest inorganic fertilizers. The time required for an analysis can be further shortened by using “Autopettes” for dispensing the standard acid and a “Titralyzer” for back titrations.
Diethylnitrosamine and Other N-Nitrosamines in Foods
Authors: Sen N P , Smith Dorothy C , Schwinghamer L , Marleau J J 
Published: February 2020

Abstract
Dimethyl-, diethyl-, di-n-propyl, and other nitrosamines in foods are determined semiquantitatively as follows: (a) initial extraction of the nitrosamines from foods into suitable solvents, (b) isolation of the nitrosamines from other interfering materials by steam distillation and ion exchange cleanup, (c) detection and semiquantitative estimation by TLC, and (d) final identification by GLC analysis of the separated compounds. The detection limit for dimethylnitrosamine in foods was 0.15 ppm and for diethyl- and di-re-propylnitrosamines, 50 ppb. The method has been successfully applied to wheat flour, fish, cheese, and spinach samples.
Forensic Aspects of Cystolith Hairs of Cannabis and Other Plants
Authors: Nakamura George R 
Published: February 2020

Abstract
Cystolith hairs, important criteria for the identification of marihuana leaf fragments, occur among several dicotyledonous families, notably the Moraceae, Boraginaceae, Loasaceae, Ulmaceae, and Caimabinaceae. Since cystoliths also develop in many forms, most species can be differentiated from Cannabis only by a very close morphological examination. The Duquenois-Levine test was found useful in confirmation, since none of 82 species, many of which had hairs similar to those found on Cannabis, yielded a positive test.