Gas Chromatographic Determination of Phenolic Compounds in Drug Preparations: Collaborative Study

1972 ◽  
Vol 55 (3) ◽  
pp. 610-612 ◽  
Author(s):  
Carol C Douglas
Keyword(s):  
Phenolic Compounds ◽  
Methyl Salicylate ◽  
Chromatographic Method ◽  
Collaborative Study ◽  
Chromatographic Determination ◽  
The Other ◽  
Gas Chromatographic Method

Abstract A gas chromatographic method for the determination of phenol, methyl salicylate, menthol , and camphor in drug preparations was studied collaboratively by 9 laboratories. Mean recoveries were: phenol 98.2, 106.0, a n d 103.6%; methyl salicylate 103.9, 102.0, and 101.9%; menthol 102.9 and 100.9%; and camphor 101.9 and 100.9%. The method has been adopted as official first action for camphor-containing drugs. Additional study will be done to improve recoveries for the other 3 compounds.

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.

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.

Gas Chromatographic Determination of Mono- and Diglycerides in Fats and Oils: Summary of Collaborative Study

1994 ◽  
Vol 77 (3) ◽  
pp. 677-680 ◽  
Author(s):  
David Firestone
Keyword(s):  
Chromatographic Method ◽  
Collaborative Study ◽  
Fats And Oils ◽  
Chromatographic Determination ◽  
Study Results ◽  
Sunflower Oils ◽  
Aoac Method ◽  
Materials Used ◽  
Gas Chromatographic Method

Abstract A collaborative study was conducted on a capillary gas chromatographic method for the determination of mono- and diglycerides in fats and oils. Other components of fats and oils such as glycerol, fatty acids, and sterols may be analyzed by this method. Six materials used in the study consisted of 2 commercial mono- and diglyceride emulsifiers, 2 synthetic compositions with known amounts of monoand diglycerides in the presence of an excess of triglycerides, and 2 refined sunflower oils spiked with mono- and diglycerides. Eight laboratories participated in the study. On the basis of the collaborative study results, the method has been adopted first action by AOAC INTERNATIONAL as an IUPAC/AOCS/AOAC method.

scholarly journals Gas Chromatographic Determination of Azoxystrobin, Fluazinam, Kresoxim-Methyl, Mepanipyrim, and Tetraconazole in Grapes, Must, and Wine

1998 ◽  
Vol 81 (6) ◽  
pp. 1185-1189 ◽  
Author(s):  
Paolo Cabras ◽  
Alberto Angion ◽  
Vincenzo L Garau ◽  
Filippo M Pirisi ◽  
Vincenzo Brandolini
Keyword(s):  
Chromatographic Method ◽  
High Selectivity ◽  
Chromatographic Determination ◽  
Mass Spectrometric ◽  
The Other ◽  
Coefficients Of Variation ◽  
Gas Chromatographic Method ◽  
Nitrogen Phosphorus ◽  
Acetone Hexane

Abstract Azoxystrobin, fluazinam, kresoxim-methyl, mepanipyrim, and tetraconazole were determined in grapes, must, and wine by a gas chromatographic method with nitrogen-phosphorus (NP) and mass spectrometric (MS) detectors. Pesticides were isolated from the matrixes by online microextraction with acetone-hexane (50 + 50, v/v). Because of the high selectivity of NP and MS detectors, no interfered peaks were present and no cleanup was necessary. Recoveries from fortified grapes, must, and wine ranged from 80 to 111 %, with coefficients of variation ranging from 1 to 14%. Limits of determination were 0.05 mg/kg for kresoxim-methyl and 0.10 mg/kg for the other compounds.

Gas Chromatographic Determination of Pentachlorophenol in Gelatin: Collaborative Study

1985 ◽  
Vol 68 (3) ◽  
pp. 419-421
Author(s):  
George Yip
Keyword(s):  
Gas Chromatography ◽  
Coefficient Of Variation ◽  
Chromatographic Method ◽  
Collaborative Study ◽  
Chromatographic Determination ◽  
Coefficients Of Variation ◽  
Gas Chromatographic Method ◽  
Hydrolysis Of ◽  
Ppm Level

Abstract Eleven collaborators participated in this study of a gas chromatographic method for the determination of pentachlorophenol (PCP) in gelatin. Following acid hydrolysis of a 2 g sample, PCP is extracted with hexane and partitioned into KOH solution. After reacidification, PCP is again extracted with hexane for determination by electron capture gas chromatography on a 1 % SP-1240DA column. Three duplicate practice samples (0.0, 0.5, and 1.5 ppm) and 5 blind duplicate collaborative samples (0.0, 0.02, 0.1, 0.5, and 2.0 ppm) were analyzed by each collaborator. Mean recoveries of PCP in the collaborative samples ranged from 88% at the 0.02 ppm fortification level to 102% at the 0.1 ppm level; the overall mean recovery was 96%. Interlaboratory coefficients of variation ranged from 16.4% for the 0.1 ppm fortification level to 22.9% for the 0.5 ppm level; the overall interlaboratory coefficient of variation was 19.5%. The method has been adopted official first action.

Gas Chromatographic Determination of N-Butyl-N-ethyl-α,α,α-trifluoro-2,6-dinitro-p-toluidine and α,α,α-Trifluoro-2,6-dinitro-N,N-dipropyl-p-toluidine in Formulations

1971 ◽  
Vol 54 (3) ◽  
pp. 711-712
Author(s):  
Martha Fuzesi
Keyword(s):  
Gas Chromatography ◽  
Quantitative Determination ◽  
Electron Capture ◽  
Chromatographic Method ◽  
Chromatographic Determination ◽  
Electron Capture Detector ◽  
Reference Solution ◽  
Gas Chromatographic Method

Abstract A gas chromatographic method is described for the quantitative determination of N-butyl-N-ethyl-α,α,α-trifluoro-2,6-dinitro-p-tolindine and α,α,α-trifluoro-2,6-dinitro-N,N-dipropyI-p-toluidine herbicides in formulations. The sample is extracted with benzene, and equal amounts of sample and reference solution in the same concentration range are analyzed by gas chromatography, using an electron capture detector and an SE-30/Diatoport S column. The method has been applied successfully to laboratory-prepared and commercial samples.

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.

scholarly journals Gas Chromatographic Determination of Chlorothalonil in Leaves and Roots of Scrophularia and in Soil

1996 ◽  
Vol 79 (2) ◽  
pp. 587-588 ◽  
Author(s):  
Lan Zhao ◽  
De-Fang Fan
Keyword(s):  
Electron Capture ◽  
Chromatographic Method ◽  
Detection Limits ◽  
Chromatographic Determination ◽  
Soil Samples ◽  
Florisil Column ◽  
Glass Column ◽  
Leaves And Roots ◽  
Gas Chromatographic Method

Abstract A gas chromatographic method is described for determination of chlorothalonil residues in leaves and roots of Scrophularia and in soil. Samples were extracted with acetone and cleaned up on a Florisil column. Chlorothalonil residues are chromatographed directly on a glass column of 1.5% OV-17 and 2% QF-1 coated on 80-100 mesh Chromosorb W (HP) support and measured with a 63Ni electron capture detector. Detection limits are 0.001 ppm for leaf, 0.005 ppm for root, and 0.001 ppm for soil.

Capillary Column Gas Chromatographic Determination of Trace Residues of the Herbicide Chlorsulfuron in Agricultural Runoff Water

1987 ◽  
Vol 70 (4) ◽  
pp. 745-748
Author(s):  
Uaz Ahmad
Keyword(s):  
Gas Chromatography ◽  
Chromatographic Method ◽  
Capillary Column ◽  
Methylene Chloride ◽  
Chromatographic Determination ◽  
Agricultural Runoff ◽  
Runoff Water ◽  
Florisil Column ◽  
Gas Chromatographic Method

Abstract A capillary column gas chromatographic method is described for determining parts-per-trillion (ppt) levels of chlorsulfuron in agricultural runoff water. The water sample is acidified with acetic acid and extracted with methylene chloride. The chlorsulfuron in the extract is derivatized to its monomethyl derivative. After Florisil column cleanup, the methylated chlorsulfuron is determined by electron-capture gas chromatography. Recovery of chlorsulfuron from fortified water samples is greater than 80%. Detection limit of the method is 25 ng chlorsulfuron/L water (25 ppt). There are 2 reaction sites on the chlorsulfuron molecule, both of which are susceptible to methylation leading to monomethyl chlorsulfuron and dimethyl chlorsulfuron. A procedure is described to methylate selectively the sulfonamide nitrogen of chlorsulfuron.

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