Collaborative Study of the Determination of Dithiocarbamate Residues by a Modified Carbon Disulfide Evolution Method

1971 ◽  
Vol 54 (3) ◽  
pp. 528-532 ◽  
Author(s):  
George E Keppel
Keyword(s):  
Hydrogen Sulfide ◽  
Stannous Chloride ◽  
Collaborative Study ◽  
The Other ◽  
Dilute Acid ◽  
Trap Hydrogen ◽  
Modified Method ◽  
Coefficients Of Variation ◽  
Naoh Solution

Abstract A modified method for determination of dithiocarbamate residue recoveries from grain was studied collaboratively. In this method dilute acid with stannous chloride is added to the crop, which is then heated to boiling for the dithiocarbamate decomposition step. A mixture of NaOH solution and benzene is used to trap hydrogen sulfide and other volatile interferences. Collaborative results were low and erratic, with large coefficients of variation. The results of the Associate Referee, on the other hand, were better. Further study on this method is recommended.

Gas Chromatographic Methods for Determination of γ-BHC in Technical Emulsifiable Concentrates and Water-Dispersible Powder Formulations and in Lindane Shampoo and Lotion: Collaborative Study

1984 ◽  
Vol 67 (4) ◽  
pp. 834-837
Author(s):  
James W Miles ◽  
Dwight L Mount ◽  
◽  
T J Beckmann ◽  
S K Carrigan ◽  
...  
Keyword(s):  
Coefficient Of Variation ◽  
Collaborative Study ◽  
Internal Standard ◽  
The Other ◽  
Water Dispersible ◽  
Coefficients Of Variation ◽  
Aoac Method ◽  
Liquid Chromatographic ◽  
Gas Chromatographic Separation

Abstract Although the gas chromatographic separation of the isomers of BHC was demonstrated two decades ago, the present AOAC method of analysis of BHC for gamma-isomer (lindane) content is based on a separation carried out on a liquid chromatographic partition column. A method of analysis has been developed that uses an OV-210 column for separation of the gamma-isomer from the other isomers and impurities in technical BHC. Di-n-propyl phthalate was chosen as an internal standard. The same system allows quantitation of lindane in lotion and shampoo after these products are extracted with ethyl acetate-isooctane (1 + 4). The analytical methods were subjected to a collaborative trial with 10 laboratories. The coefficient of variation for technical BHC was 2.83%. For the water-dispersible powder and emulsifiable concentrate, the coefficients of variation were 2.89% and 4.62%, respectively. Coefficients of variation for 1% lindane lotion and shampoo were 4.36% and 11.92%, respectively. The method has been adopted official first action.

Collaborative Study of the Determination of Sorbic Acid in Wine

1975 ◽  
Vol 58 (1) ◽  
pp. 133-135
Author(s):  
Arthur Caputi ◽  
Karen Slinkard
Keyword(s):  
Sorbic Acid ◽  
Collaborative Study ◽  
Thiobarbituric Acid ◽  
The Other ◽  
Ultraviolet Spectrophotometry ◽  
Acid Complex ◽  
Average Recovery ◽  
Colorimetric Measurement ◽  
Coefficients Of Variation

Abstract Eleven collaborators participated in a study of 2 methods for determining sorbic acid in wine. One method utilizes ultraviolet spectrophotometry and the other depends on the colorimetric measurement of a thiobarbituric acid complex. Three different wine types were each spiked with 200, 300, and 400 mg sorbic acid/ L. Average recovery ranged from 97.3 to 107.5% with the thiobarbituric acid method with coefficients of variation from 4.4 to 8.7%. The ultraviolet method gave recoveries from 97 to 103.5% with coefficients of variation ranging from 2.0 to 6.4%. Comments on both methods from collaborators were favorable. Both methods have been adopted as official first action.

Microbiological Assay of Streptomycin in Feeds: 1971 Collaborative Study

1972 ◽  
Vol 55 (4) ◽  
pp. 714-717
Author(s):  
John J Mayernik ◽  
Gloria Y Fiori ◽  
Shirley Hughes
Keyword(s):  
Sample Size ◽  
Reference Point ◽  
Collaborative Study ◽  
Microbiological Assay ◽  
Modified Method ◽  
Coefficients Of Variation ◽  
Aoac Official ◽  
Low Levels

Abstract The AOAC official first action method for the determination of streptomycin in feed in which the regular streptomycin assay agar is used was modified for application to the assay of low levels of streptomycin. The modifications consist of (1) increasing the sample size, (2) reducing the amount of agar in the assay plates, (3) lowering the concentration of the reference point on the assay plates, and (4) incubating the plates at 22–25°C instead of 37°C. Fifteen collaborators used the modified method to assay 6 feeds containing 5–30 g streptomycin/ ton. Mean recoveries ranged from 91.7 to 111.0% and coefficients of variation ranged from 5.8 to 8.7%. The method modified as described has been adopted as official first action for the assay of feeds containing 5–30 g streptomycin/ton.

Collaborative Study of a Modified Method for the Determination of Aflatoxins in Copra, Copra Meal, and Coconut

1971 ◽  
Vol 54 (4) ◽  
pp. 874-878
Author(s):  
F J Baur ◽  
J C Armstrong
Keyword(s):  
Aflatoxin B1 ◽  
Quantitative Measurement ◽  
Collaborative Study ◽  
Copra Meal ◽  
Modified Method

Abstract A collaborative study, in which 19 laboratories participated, was conducted on a modified method for the determination of aflatoxins in 2 copra samples, one naturally contaminated, and 4 samples of naturally contaminated copra meal. The sensitivity and precision of the modified method for aflatoxin B1 and total aflatoxins were comparable to the official methods for peanuts and peanut products. Aflatoxins B2, G1, and G2 were reported by most of the laboratories, but background interferences made quantitative measurement less reliable than for B1. The method as it presently stands is also applicable to the analysis of coconut. The method has been adopted as official first action; further study will be directed toward improved precision for analysis of aflatoxins B2, G1, and G2.

Multiresidue Gas Chromatographic Method for Determining Organochlorine Pesticides in Poultry Fat: Collaborative Study

1984 ◽  
Vol 67 (2) ◽  
pp. 284-289 ◽  
Author(s):  
James A Ault ◽  
Tim E Spurgeon ◽  
◽  
M M Anderson ◽  
R Bowers ◽  
...  
Keyword(s):  
Chromatographic Method ◽  
Collaborative Study ◽  
Gel Permeation Chromatography ◽  
Accuracy And Precision ◽  
Coefficients Of Variation ◽  
Poultry Fat ◽  
Gel Permeation ◽  
Detector Method ◽  
Gas Chromatographic Method

Abstract A gas chromatographic electron capture detector method is described for the quantitative determination of organochlorine pesticide residues in poultry fat. The samples are rendered and cleaned up using automated gel permeation chromatography. The collaborative samples consisted of 10 fortified samples and one incurred residue sample, all in duplicate. Fortification levels ranged from 0.15 to 1.0 ppm for a-BHC, lindane, cis- and frans-chlordane, octachlor epoxide, o,p' and p,p'-DDT, p,p'-DDE, p,p'-TDE, hexachlorobenzene, heptachlor epoxide, dieldrin, endrin, methoxychlor, mirex, and toxaphene. The average recovery was 91.9% with a range of 81-102%. The ranges of coefficients of variation were: CVo = 3.39-14.79%; CVL = 0-16.6%; and CVx = 5.82-19.0%. The results indicate accuracy and precision comparable to other official methodology. The method has been adopted official first action.

Collaborative Study of a Semiautomated Fluorometric Method for the Determination of Reserpine in Tablets

1976 ◽  
Vol 59 (2) ◽  
pp. 289-292
Author(s):  
Mary A Kreienbaum
Keyword(s):  
Vanadium Pentoxide ◽  
Collaborative Study ◽  
Dosage Level ◽  
Fluorometric Method ◽  
Coefficients Of Variation ◽  
Semiautomated Method

Abstract A semiautomated fluorometric method for the determination of resperpine in tablets was collaboratively studied by 7 laboratories. The method is a modification of the semiautomated method of Urbányi and Stober, which involves formation of a fluorogen with vanadium pentoxide. Collaborators were supplied with 3 composites, each from a different dosage level of commercial tablets. The results obtained agreed well with the AOAC manual fluorometric method; coefficients of variation ranged from 0.45 to 2.70%. The method has been adopted as official first action.

Automated Method for the Determination of Niacin and Niacinamide in Cereal Products: Collaborative Study

1975 ◽  
Vol 58 (4) ◽  
pp. 799-803
Author(s):  
Anthony F Gross
Keyword(s):  
Chemical Method ◽  
Collaborative Study ◽  
Pet Food ◽  
Microbiological Method ◽  
Chemical Methods ◽  
Cereal Products ◽  
Automated Method ◽  
Coefficients Of Variation ◽  
Baked Products

Abstract In a collaborative study, an automated method for the determination of niacin and niacinamide in cereal products was compared with the official final action microbiological (43.121–43.125) and chemical (43.044–43.046) methods. Ten samples of cereal products, including enriched flour, yeast-leavened baked products, fortified breakfast cereals, and baked pet food products, were submitted to 14 laboratories. Nine laboratories reported values by the automated method, 6 reported values by the microbiological method, and 7 reported values by the chemical method. The results from the microbiological method were not subjected to analysis of variance because of the unusually large between-laboratory variation. The between-laboratory coefficients of variation for the automated and chemical methods were 10.90 and 10.18%, on the basis of results from 7 and 4 laboratories, respectively. There was no significant (p>0.05) difference between methods when results from the 4 laboratories who used both methods were compared. The automated chemical method has been adopted as official first action.

Gas-Liquid Chromatographic Determination of Tetradif on Technical and Formulations: Collaborative Study

1981 ◽  
Vol 64 (4) ◽  
pp. 829-832
Author(s):  
Bram Van Rossum ◽  
Albertus Martijn ◽  
James E Launer ◽  
◽  
E C Calamita ◽  
...  
Keyword(s):  
Collaborative Study ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Flame Ionization ◽  
Coefficients Of Variation ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract The gas-liquid chromatographic determination of tetradifon technical and formulations was collaboratively studied in duplicate with 12 laboratories. Six samples were dissolved in dichloroethane with n-hexacosane as the internal standard, chromatographed on a column of 3% SE-52, and detected by flame ionization. The average coefficients of variation were 1.2% for the 2 technical samples, 1.6% for the 2 wettable powders, and 1.5% for the 2 emulsifiable concentrates. The method has been adopted official first action.

scholarly journals Determination of Cholecalciferol (Vitamin D3) in Selected Foods by Liquid Chromatography: NMKL Collaborative Study

2003 ◽  
Vol 86 (2) ◽  
pp. 400-406 ◽  
Author(s):  
Anders Staffas ◽  
Arne Nyman ◽  
K Ask ◽  
E Hermansson ◽  
J S Jacobsen ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Standard Deviation ◽  
Fish Oil ◽  
Vitamin D3 ◽  
Collaborative Study ◽  
The Other ◽  
Vitamin D2 ◽  
Cooking Oil ◽  
Relative Standard

Abstract Results are presented from an NMKL (Nordic Committee on Food Analysis) collaborative study of a method for the determination of cholecalciferol (vitamin D3) in foods. The method is based on the addition of an internal standard (vitamin D2), followed by saponification and extraction with n-heptane. The fraction that contains vitamin D2/D3 is separated by preparative normal-phase liquid chromatography (LC), and the analytes are determined by reversed-phase LC with UV detection at 265 nm. The method was tested by 8 participating laboratories. In this study 6 different matrixes were analyzed for cholecalciferol content: milk, liquid infant formula (gruel), cooking oil, margarine, infant formula, and fish oil. The contents varied from 0.4 to 12 μg/100 g. Three matrixes (milk, gruel, and margarine) were fortified with vitamin D3. In the other matrixes, vitamin D3 was added at 3 different levels at the Swedish National Food Administration. The milk was analyzed as a blind duplicate, whereas the other matrixes were analyzed as split-level pairs. The recoveries from the samples with vitamin D3 added varied from 93 to 102%. The repeatability relative standard deviation (RSDr) values for accepted results varied between 2.2% (fish oil) and 7.4% (cooking oil), whereas the reproducibility relative standard deviation (RSDR) values varied between 6.8% (margarine) and 24% (cooking oil).

Liquid Chromatographic Determination of Triadimefon in Technical and Formulated Products: Collaborative Study

1985 ◽  
Vol 68 (3) ◽  
pp. 586-589
Author(s):  
Stephen C Slahck
Keyword(s):  
Collaborative Study ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Normal Phase ◽  
Coefficients Of Variation ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Technical Products

Abstract A liquid chromatographic method for the determination of triadimefon (Bayleton™) in triadimefon technical and formulated products has been developed and subjected to a collaborative study with 7 participating collaborators. Formulations were extracted with mobile solvent and analyzed by normal phase chromatography, with 4-chlorophenyl sulfoxide as an internal standard. Collaborators were furnished with standards and samples of technical products, 50% wettable powders, and 25% wettable powders for analysis. Coefficients of variation of the values obtained on these samples were 1.42, 0.82, and 1.05%, respectively. The method has been adopted official first action.

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