Gas Chromatographic Separation and Quantitative Estimation of Barbiturate Mixtures in Solid Dosage Forms

1968 ◽  
Vol 51 (3) ◽  
pp. 619-621
Author(s):  
John L Allen
Keyword(s):  
Chromatographic Separation ◽  
Chromatographic Method ◽  
Quantitative Estimation ◽  
Collaborative Study ◽  
Internal Standard ◽  
Dosage Forms ◽  
Solid Dosage Forms ◽  
Solid Dosage ◽  
Gas Chromatographic Method ◽  
Gas Chromatographic Separation

Abstract A gas chromatographic method has been described for the analysis of mixed barbiturates in solid dosage forms. Analysis on a 10% SE-30 column gave good separations for butabarbital, amobarbital, secobarbital, pentobarbital, and/or phenobarbital; amobarbital is not separated adequately from pentobarbital. An internal standard, mephobarbital, is used to minimize injection errors. The method gives both good quantitative and qualitative results on the barbiturates investigated. Two synthetic tablet mixtures were analyzed by this procedure and recoveries were 98—103%. It is recommended that the method be subjected to collaborative study.

Modification of the AOAC Gas-Liquid Chromatographic Method for Indole in Shrimp: Collaborative Study

1982 ◽  
Vol 65 (4) ◽  
pp. 842-845
Author(s):  
Theodore L Chambers ◽  
◽  
E C Netz ◽  
K Ogger
Keyword(s):  
Silica Gel ◽  
Chromatographic Method ◽  
Collaborative Study ◽  
Internal Standard ◽  
Current Method ◽  
Peak Height ◽  
Modified Method ◽  
Liquid Chromatographic Method ◽  
Gas Chromatographic Method ◽  
Liquid Chromatographic

Abstract Several changes were suggested for standardization of the AOAC official final action gas chromatographic method for the determination of indole in shrimp. In a collaborative study, 3 FDA laboratories compared the modified method with the current method. At a 95% confidence level, the same results were obtained for each respective sample by the AOAC or the modified method, which had the following changes. The cleanup column was standardized by drying the silica gel for 2 h at 125°C and equilibrating with 3 g of water/25 g of silica gel. Concentrated ethyl acetate shrimp extracts were treated with anhydrous sodium sulfate before column cleanup and indole was eluted from the column with 15% ethyl ether/hexane. A reduced amount of the internal standard, 2-methylindole, was used to improve peak height measurements at the 25 μg% indole level. The modified method has been adopted official first action to replace method 18.075.

Gas Chromatographic Method for Determination of Cypermethrin in Pesticide Formulations: Collaborative Study

1987 ◽  
Vol 70 (1) ◽  
pp. 51-53
Author(s):  
J F C Tyler
Keyword(s):  
Chromatographic Method ◽  
Collaborative Study ◽  
Internal Standard ◽  
Coefficients Of Variation ◽  
Pesticide Formulations ◽  
Glass Column ◽  
Technical Material ◽  
Gas Chromatographic Method ◽  
Ethylhexyl Phthalate

Abstract A gas chromatographic method for determination of total cypermethrin in technical and formulated products has been developed and subjected to a collaborative study involving IS participating laboratories. Each sample was dissolved in methyl isobutyl ketone containing di(2-ethylhexyl) phthalate as internal standard and analyzed by gas chromatography on a glass column with 3% OV-101 on Chromosorb W-HP. Each collaborator was furnished with reference stdard and 4 samples of technical material, 3 emulsifiable concentrates, one wettable powder, and one ultralow volume formulation for analysis. The coefficients of variation of the results obtained ranged from 0.955 to 1.7462%. The method has been adopted as official first action by AOAC.

Gas Chromatographic Method for Determination of Permethrin in Pesticide Formulations: Collaborative Study

1987 ◽  
Vol 70 (1) ◽  
pp. 53-55
Author(s):  
J F C Tyler
Keyword(s):  
Chromatographic Method ◽  
Collaborative Study ◽  
Internal Standard ◽  
Isobutyl Ketone ◽  
Coefficients Of Variation ◽  
Pesticide Formulations ◽  
Glass Column ◽  
Technical Material ◽  
Gas Chromatographic Method

Abstract A gas chromatographic method for determination of permethrin in technical and formulated products has been developed and subjected to a collaborative study involving 19 participating laboratories. Each sample was dissolved in methyl isobutyl ketone containing n-octacosane as internal standard and analyzed by gas chromatography on a glass column with 3% OV-210 on Chromosorb W-HP. Each collaborator was furnished with reference standard and 5 samples of technical material (90-95%), 8 emulsifiable concentrates (10-50%), 2 wettable powders (20-30%), one dustable powder (1-2%), and one mter-dispersible granules (1-2%) for analysis. The coefficients of variation of the results obtained ranged from 0.79 to 4.24%. The method has been adopted as official first action by AOAC.

scholarly journals Gas Chromatographic Determination of Alachlor in Microencapsulated Formulations: Mini-Collaborative Study

1987 ◽  
Vol 70 (6) ◽  
pp. 1056-1058
Author(s):  
David F Tomkins
Keyword(s):  
Coefficient Of Variation ◽  
Chromatographic Method ◽  
Collaborative Study ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Chromatographic Column ◽  
Data Points ◽  
Gas Chromatographic Method ◽  
Isothermal Gas

Abstract An isothermal gas chromatographic method for measuring alachlor in Micro-Tech® (microencapsulated) formulations was tested by 5 collaborators. The samples were prepared in acetone, and alachlor was determined using a gas chromatographic column of 10% SP- 2250 on 100-120 mesh Supelcoport. Di-n-pentylphthalate was used as the internal standard. Collaborators made single determinations on 5 samples distributed as blind duplicates. The mini-collaborative study generated 47 data points. The coefficient of variation (CV„- pooled) was 1.35%, and CVx-pooled was 0.73%. The method was simple to use and did not reveal any interferences in samples tested. The method has been adopted official first action as an AOACCIPAC method.

Gas Chromatographic Determination of Fensulfothion in Formulations: Collaborative Study

1986 ◽  
Vol 69 (3) ◽  
pp. 488-490
Author(s):  
William R Betker ◽  
◽  
E W Balcer ◽  
O O Bennett ◽  
W R Coffman ◽  
...  
Keyword(s):  
Chromatographic Method ◽  
Methylene Chloride ◽  
Collaborative Study ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Gas Chromatograph ◽  
Technical Product ◽  
Coefficients Of Variation ◽  
Gas Chromatographic Method

Abstract A collaborative study was conducted on a gas chromatographic method for determination of fensulfothion. Eleven laboratories analyzed 2 technical and two 6 lb/U.S. gal. spray concentrate samples. In the analysis, samples are dissolved in methylene chloride which contains 4-chlorophenyl sulfoxide as an internal standard, and solutions are injected into a gas chromatograph equipped with an OV-330 column. Withinlaboratory repeatability was 0.79% for technical product and 0.37% for the spray concentrate samples, with coefficients of variation of 0.88 and 0.58%, respectively. Among-laboratories reproducibility was 0.81% for technical product and 0.53% for the spray concentrate, with coefficients of variation of 0.91 and 0.84%, respectively. The method has been adopted official first action.

Headspace Gas Chromatographic Method for Determination of Ethanol in Canned Salmon: Collaborative Study

1986 ◽  
Vol 69 (3) ◽  
pp. 524-526
Author(s):  
Thomas A Hollingworth ◽  
Harold R Throm ◽  
Marleen M Wekell ◽  
William F Trager ◽  
Michael W O’Donnell ◽  
...  
Keyword(s):  
Chromatographic Method ◽  
Collaborative Study ◽  
Internal Standard ◽  
Sampling Technique ◽  
Flame Ionization ◽  
Coefficients Of Variation ◽  
Headspace Gas ◽  
The Mean ◽  
Gas Chromatographic Method

Abstract Six laboratories collaboratively studied a headspace gas chromatographic method for determination of ethanol in the aqueous phase of canned salmon. Ethanol is determined by a headspace sampling technique with tert-butanol as the internal standard, using a gas chromatograph equipped with a Super Q column and a flame ionization detector. With outliers excluded, the mean recoveries from samples spiked with 25.1 and 78.4 ppm ethanol were 112 and 110%, respectively. For the 4 sample pairs quantitated, repeatability coefficients of variation ranged from 1.42 to 4.25% and reproducibility coefficients of variation from 2.55 to 8.09%, with 3 of the 4 reported values less than 5%. The method has been adopted official first action.

Collaborative Study of a Gas Chromatographic Method for Phenothiazine in Drugs

1967 ◽  
Vol 50 (3) ◽  
pp. 682-684
Author(s):  
C L Bramlett
Keyword(s):  
Chromatographic Method ◽  
Collaborative Study ◽  
Chloroform Solution ◽  
Internal Standard ◽  
Ground Sample ◽  
Gas Chromatographic Method

Abstract A rapid and specific gas chromatographic method for phenothiazine in microgram amounts has been developed and studied collaboralively. The phenothiazine is extracted from a ground sample with chloroform. An internal standard, promethazine hydrochloridc, is added to the extract and to a chloroform solution of phenothiazine standard. Both solutions are diluted and aliquots are chromatographed on a 4' column of Gas Chrom Q with a 5% coating of Apiezon L. Collaborative results, based on 18 separate analyses of each sample, were 38.2 ± 1.2% (38.2% added), and 42.2 ± 1.2% (43.1% added)

Gas Chromatographic Determination of Isofenphos in Technical and Formulated Products: Collaborative Study

1987 ◽  
Vol 70 (1) ◽  
pp. 55-57
Author(s):  
Daniel E Terry
Keyword(s):  
Thermal Conductivity ◽  
Gas Chromatography ◽  
Chromatographic Method ◽  
Collaborative Study ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Flame Ionization ◽  
Coefficients Of Variation ◽  
Gas Chromatographic Method

Abstract A gas chromatographic method for the determination of isofenphos (OFTANOL®) in isofenphos technical and liquid formulations has been developed and collaboratively studied by 11 laboratories. Two technical samples and 2 liquid flowable samples were analyzed after shaking/extracting in methanol which contained diisobutyl phthalate as an internal standard. The extracts were analyzed by gas chromatography using an SP-2100 column and either flame ionization or thermal conductivity detection. Coefficients of variation were 0.57 and 1.27% for the technical and formulated products, respectively. The GC method has been adopted official first action as a AOACCTPAC method.

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