Differential Pulse Polarographic Determination of Iodine in Thyroid Tablets: Collaborative Study

1982 ◽  
Vol 65 (5) ◽  
pp. 1059-1062
Author(s):  
Walter Holak ◽  
◽  
R Baetz ◽  
P Beavin ◽  
P Gable ◽  
...  
Keyword(s):  
Collaborative Study ◽  
Differential Pulse ◽  
Polarographic Determination ◽  
Coefficients Of Variation ◽  
Repeatability And Reproducibility ◽  
Standard Deviations ◽  
The U.S

Abstract A differential pulse polarographic (DPP) method for the determination of iodine in thyroid and thyroid preparations was collaboratively studied by 8 laboratories. The overall concentration of iodine in commercial thyroid tablets containing ¼, 1,2, and 5 gr. of declared thyroid was 0.196%. The overall repeatability and reproducibility standard deviations were 0.0043 and 0.0067, respectively, and the corresponding coefficients of variation were 2.18 and 3.41%, respectively. The results obtained by the DPP method agreed with those obtained by the U.S. Pharmacopeia XX method at the various concentrations of declared thyroid studied. The DPP method has been adopted official first action.

Liquid Chromatographic Method for Determination of Iodine in Milk: Collaborative Study

1993 ◽  
Vol 76 (4) ◽  
pp. 711-719 ◽  
Author(s):  
David Sertl ◽  
William Malone ◽  
◽  
P Beljaars ◽  
C Blake ◽  
...  
Keyword(s):  
Membrane Filter ◽  
Collaborative Study ◽  
Reversed Phase ◽  
Powdered Milk ◽  
Insoluble Material ◽  
Relative Standard ◽  
Repeatability And Reproducibility ◽  
Standard Deviations ◽  
Liquid Chromatographic

Abstract Nine laboratories participated in an AOAC International/ International Dairy Federation collaborative study on a liquid chromatographic (LC) method for determination of iodine in milk. Liquid milk is passed through a 25 000 MW membrane filter to remove protein and insoluble material. Iodine (in the form of iodide) in the clear filtrate is separated by reversed-phase ion-pair LC and is detected electrochemically. Participants analyzed 2 commercial pasteurized whole milks and 5 nonfat dry milk powders in blind duplicate. Each sample was tested in duplicate on 2 days. Repeatability and reproducibility standard deviations (sr and SR, respectively) and repeatability and reproducibility relative standard deviations (RSDr and RSDR, respectively) for determinations of iodine in whole milk (mean recovery, 86.7%) were as follows: sr, 22 μg/L; SR, 22 μg/L; RSDr, 8.2%; and RSDR, 8.3%. For powdered milk (mean recovery, 91 %), the values were as follows: sr, 0.14 μg/g; SR, 0.22 μg/g; RSDr, 9.0%; and RSDR, 12.7%. The method was adopted first action by AOAC International.

Determination of Dextran in Raw Cane Sugar by Roberts Copper Method: Collaborative Study

1988 ◽  
Vol 71 (2) ◽  
pp. 276-279
Author(s):  
Margaret A Clarke ◽  
Mary An Godshall
Keyword(s):  
Collaborative Study ◽  
Cane Sugar ◽  
Coefficients Of Variation ◽  
Raw Sugar ◽  
Repeatability And Reproducibility

Abstract A collaborative study was conducted using the Roberts copper method for the determination of dextran in raw cane sugars. Four samples were analyzed in duplicate, representing the range of dextran concentrations found in raw sugar. The overall repeatability and reproducibility coefficients of variation were 4.3 and 13.2%, respectively. The method has been adopted official first action.

Determination of N-Nitrosodimethylamine in Nonfat Dry Milk: Collaborative Study

1984 ◽  
Vol 67 (2) ◽  
pp. 232-236
Author(s):  
Nrisinha P Sen ◽  
Stephen Seaman ◽  
K Karpinsky ◽  
◽  
M Castegnaro ◽  
...  
Keyword(s):  
Thermal Energy ◽  
Collaborative Study ◽  
Sulfamic Acid ◽  
Complete Data ◽  
Energy Analyzer ◽  
Coefficients Of Variation ◽  
Dry Milk ◽  
Repeatability And Reproducibility ◽  
Nonfat Dry Milk

Abstract Ten laboratories participated in a collaborative study of a method for the determination of JV-nitrosodimethylamine (NDMA) in nonfat dry milk. NDMA is eluted with dichloromethane from a mixture of Celite, acidic sulfamic acid, and nonfat dry milk (all packed in a chromatography column), concentrated in a Kuderna-Danish concentrator, and finally analyzed by a GC-thermal energy analyzer technique. Ten samples were studied: 6 were naturally contaminated (NDMA levels 0.38- 3.56 ppb) and 4 were spiked with known levels (0.96 and 3.2 ppb) of NDMA. The coefficients of variation (CV) of the complete data for the naturally contaminated samples (excluding the 2 samples containing the lowest levels) were 8.5% and 22.5% for repeatability and reproducibility, respectively. The corresponding CVs for the spiked samples were 14.4% and 20.4%, respectively. The percent recoveries of the added NDMA in the spiked samples (at the 2 levels indicated above) were 101.6 ± 3.2 (omitting 1 outlier) and 95 ∓ 2.1, respectively. The method has been adopted official first action.

scholarly journals Determination of Fumonisins B1 and B2 in Corn and Corn Flakes by Liquid Chromatography with Immunoaffinity Column Cleanup: Collaborative Study

2001 ◽  
Vol 84 (6) ◽  
pp. 1828-1838 ◽  
Author(s):  
Angelo Visconti ◽  
Michele Solfrizzo ◽  
Annalisa De Girolamo ◽  
H Bresch ◽  
P Burdaspal ◽  
...  
Keyword(s):  
Collaborative Study ◽  
Immunoaffinity Column ◽  
Relative Standard ◽  
Repeatability And Reproducibility ◽  
Double Extraction ◽  
Standard Deviations ◽  
Corn Flakes ◽  
Liquid Chromatographic ◽  
Fumonisins B1 And B2

Abstract A liquid chromatographic (LC) method for the determination of fumonisins B1 (FB1) and B2 (FB2) in corn and corn flakes was collaboratively studied by 23 laboratories, which analyzed 5 blind duplicate pairs of each matrix to establish the accuracy, repeatability, and reproducibility characteristics of the method. Fumonisin levels in the corn ranged from <0.05 (blank) to 1.41 μg/g for FB1 and from <0.05 to 0.56 μg/g for FB2, whereas in the corn flakes they ranged from <0.05 to 1.05 μg/g for FB1 and from <0.05 to 0.46 μg/g for FB2. The method involved double extraction with acetonitrile–methanol–water (25 + 25 + 50), cleanup through an immunoaffinity column, and LC determination of the fumonisins after derivatization with o-phthaldialdehyde. Relative standard deviations for the within-laboratory repeatability (RSDr) of the corn analyses ranged from 19 to 24% for FB1 and from 19 to 27% for FB2; for the corn flakes analyses, RSDr ranged from 9 to 21% for FB1 and from 8 to 22% for FB2. Relative standard deviations for the between-laboratories reproducibility (RSDR) of the corn analyses ranged from 22 to 28% for FB1 and from 22 to 30% for the FB2; for corn flakes analyses, RSDR ranged from 27 to 32% for FB1 and from 26 to 35% for FB2. Mean recoveries of FB1 and FB2 from corn spiked with FB1 at 0.80 μg/g and with FB2 at 0.40 μg/g were 76 and 72%, respectively; for corn flakes spiked at the same levels recoveries were 110 and 97% for FB1 and FB2, respectively. HORRAT ratios for the analyses of corn ranged from 1.44 to 1.53 for FB1 and from 0.96 to 1.48 for FB2, whereas for corn flakes they ranged from 1.60 to 1.82 for FB1 and from 1.39 to 1.68 for FB2.

Collaborative Study of the Determination of Dichlorophene in Veterinary Preparations by Ultraviolet Spectrophotometry

1972 ◽  
Vol 55 (1) ◽  
pp. 163-165
Author(s):  
Dalia M Gilvydis
Keyword(s):  
Standard Deviation ◽  
Collaborative Study ◽  
Liquid Extraction ◽  
Synthetic Mixture ◽  
Ultraviolet Spectrophotometry ◽  
Average Recovery ◽  
Liquid Liquid Extraction ◽  
Coefficients Of Variation ◽  
Standard Deviations

Abstract Dichlorophene is determined in veterinary preparations by a liquid-liquid extraction and UV quantitation. Eight collaborators each analyzed 4 commercial preparations and one synthetic mixture. The average recovery for dichlorophene in the synthetic mixture is 100.3% with a standard deviation of 2.13. The standard deviations obtained for the 5 samples range from 0.13 to 3.69 with coefficients of variation from 0.69 to 3.43. It is recommended that the method be adopted as official first action.

Comparison of Kjeldahl Method for Determination of Crude Protein in Cereal Grains and Oilseeds with Generic Combustion Method: Collaborative Study

1993 ◽  
Vol 76 (4) ◽  
pp. 780-786 ◽  
Author(s):  
Ronald C Bicsak ◽  
◽  
R Boles ◽  
R Cathey ◽  
V Collins ◽  
...  
Keyword(s):  
Crude Protein ◽  
Animal Feed ◽  
Collaborative Study ◽  
Combustion Method ◽  
Cereal Grains ◽  
Relative Standard ◽  
Kjeldahl Method ◽  
Repeatability And Reproducibility ◽  
Standard Deviations

Abstract Seven laboratories participated in a collaborative study to extend the applicability of the AOAC generic combustion method for determination of crude protein in animal feed (990.03) to include determination in cereal grains and oilseeds. In the study, method 990.03 was compared with the AOAC mercury catalyst Kjeldahl method for determination of protein in grains (979.09) and crude protein in animal feed (954.01). The study also evaluated the effect on the results of fineness of grind. For determination of crude protein in grains and oilseeds by the combustion method, standard deviations for repeatability and reproducibility ranged from 0.10 to 0.37 and from 0.25 to 0.54, respectively, and relative standard deviations for repeatability and reproducibility ranged from 0.77 to 2.57% and from 1.24 to 3.15%, respectively. The combustion method was adopted first action by AOAC International for determination of crude protein in cereal grains and oilseeds containing 0.2- 20% nitrogen.

Liquid Chromatographic Determination of Penicillin V Potassium in Tablets: Collaborative Study

1989 ◽  
Vol 72 (6) ◽  
pp. 883-884
Author(s):  
Barry Mopper
Keyword(s):  
Collaborative Study ◽  
Potassium Phosphate ◽  
Internal Standard ◽  
Photometric Detection ◽  
Penicillin V ◽  
Relative Standard ◽  
Repeatability And Reproducibility ◽  
Standard Deviations ◽  
Liquid Chromatographic

Abstract A liquid chromatographic method for the determination of penicillin V potassium in tablets was collaboratively studied by 7 laboratories. The method uses an octadecyl silane reverse-phase column, a mobile phase of acetonitrile-methanol-O.OlM potassium phosphate monobasic (21 + 4 + 75 v/v/v), photometric detection at 225 nm, and sulfadimethoxine as an internal standard. Each collaborator received 6 samples: powdered composites of 2 commercial tablet preparations and 1 synthetic tablet powder mixture, each with blind duplicates. The mean repeatability and reproducibility relative standard deviations for commercial samples were, respectively, 1.10 and 1.46% (250 mg dosage), and 0.84 and 2.82% (500 mg dosage). The average standard recovery from the synthetic formulation was 99.1%, with repeatability and reproducibility relative standard deviations of 1.30 and 3.66%, respectively. The method has been adopted official first action.

Proof Determination of Liqueurs and Alcoholic Dairy Products: Collaborative Study

1983 ◽  
Vol 66 (5) ◽  
pp. 1148-1151
Author(s):  
Duane H Strunk ◽  
Bertha M Timmel ◽  
Frances L Rapp ◽  
John C Aicken ◽  
◽  
...  
Keyword(s):  
Dairy Products ◽  
Ethanol Concentration ◽  
Collaborative Study ◽  
Dissolved Solids ◽  
Coefficients Of Variation ◽  
Sugar Mixtures ◽  
Standard Deviations

Abstract A method is described for determining the ethanol concentration of liqueur-type products containing dissolved solids. The sample is distilled in an allglass still equipped with spherical joints; the proof of the distillate, diluted to known volume, is measured by a Mettler/Paar density meter. Ten collaborators determined proof of 6 different synthetic liqueurs containing ethanol-water-sugar mixtures and 2 alcoholic dairy products. Proof of the samples varied from 33 to 92°. Standard deviations and coefficients of variation for this method varied from 0.069 to 0.278 and from 0.20° to 0.36°, respectively. The method has been adopted official first action.

High Pressure Liquid Chromatographic Determination of Glycyrrhizic Acid or Glycyrrhizic Acid Salts in Various Licorice Products: Collaborative Study

1982 ◽  
Vol 65 (3) ◽  
pp. 572-574
Author(s):  
Peter S Vora ◽  
◽  
H Estes ◽  
Dr Grigor ◽  
B Hodge ◽  
...  
Keyword(s):  
High Pressure ◽  
Glycyrrhizic Acid ◽  
Collaborative Study ◽  
Chromatographic Determination ◽  
Coefficients Of Variation ◽  
Liquid Chromatographic Determination ◽  
Repeatability And Reproducibility ◽  
Liquid Chromatographic ◽  
Acid Salts

Abstract A collaborative study determining glycyrrhizic acid or glycyrrhizic acid salts content of various licorice products has been conducted using high pressure liquid chromatography (HPLC). Five samples containing various concentrations of glycyrrhizic acid were analyzed in blind replicates by 8 collaborators. The results indicate excellent repeatability and reproducibility with coefficients of variation less than 7.5%. In addition, this method allows the determination of glycyrrhizic acid in less than 15 min compared with 3 days for the conventional gravimetric and colorimetric methods. The method has been adopted official first action.

Collaborative Study of the Colorimetric Determination of Zirconium in Antiperspirant Aerosols

1977 ◽  
Vol 60 (3) ◽  
pp. 663-668
Author(s):  
Paul Beavin
Keyword(s):  
Statistical Evaluation ◽  
Collaborative Study ◽  
Colorimetric Determination ◽  
Fusion Procedure ◽  
Coefficients Of Variation ◽  
Zirconium Compounds ◽  
Insoluble Form ◽  
Standard Deviations ◽  
Insoluble Compounds

Abstract A previously published method for determining zirconium in antiperspirant aerosols was collaboratively studied by 7 laboratories. The method consists of 2 procedures: a rapid dilution procedure for soluble zirconium compounds or a lengthier fusion procedure for total zirconium (soluble and insoluble compounds), followed by colorimetric determination. The collaborators were asked to perform the following: Spiking materials representing 4 levels of soluble zirconium were added to weighed portions of a zirconium-free cream base concentrate and the portions were assayed by the dilution procedure. Spiking materials representing 4 levels of zirconium in either the soluble or the insoluble form (or as a mixture) were also added to portions of the same concentrate and these portions were assayed by the fusion procedure. They were also asked to concentrate and assay, by both procedures, 2 cans each of 2 commercial aerosol antiperspirants containing zirconyl hydroxychloride. The average per cent recoveries and standard deviations for spiked samples were 99.8–100.2 and 1.69–2.71, respectively, for soluble compounds determined by the dilution procedure, and 93.8–97.4 and 3.09–4.78, respectively, for soluble and/or insoluble compounds determined by the fusion procedure. The average per cent zirconium found by the dilution procedure in the 2 commercial aerosol products was 0.751 and 0.792, respectively, with coefficients of variation of 2.94 and 2.53%, respectively. Insufficient collaborative results were received for the fusion procedure for statistical evaluation. The dilution procedure has been adopted as official first action.

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