Gas-Liquid Chromatographic Determination of Strychnine in Grain Baits

1975 ◽  
Vol 58 (5) ◽  
pp. 961-964 ◽  
Author(s):  
Alan R Hanks ◽  
Barbara S Engdahl ◽  
Billy M Colvin
Keyword(s):  
Internal Standard ◽  
Chromatographic Determination ◽  
Peak Height ◽  
Good Precision ◽  
Flame Ionization ◽  
Glass Column ◽  
Chromatographic Procedure ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A simple and rapid gas-liquid chromatographic procedure, using a 6’ × ¼“ glass column packed with 5% SE-30 on Chromosorb W (DMCS) and a flame ionization detector, is described. Grain baits containing strychnine alkaloid are ground, mixed, and extracted by shaking with chloroform containing an internal standard, 1,3,5-triphenylbenzene. Without further cleanup, extract nitrates are injected directly into a gas chromatograph. Peak height ratios are used for quantitation of strychnine. The analysis of commercial samples shows that the method compares well with a commonly employed ultraviolet spectrophotometric method; good precision, with recoveries ranging from 89.9 to 91.7%, is obtained in the analysis of prepared samples. The method is sensitive to 2 μg strychnine.

Gas-Liquid Chromatographic Determination of Chlorpyriphos in Dursban Insecticide Formulations

1973 ◽  
Vol 56 (5) ◽  
pp. 1093-1095
Author(s):  
Alan R Hanks ◽  
Barbara S Engdahl ◽  
Billy M Colvin
Keyword(s):  
Internal Standard ◽  
Chromatographic Determination ◽  
Peak Height ◽  
Good Precision ◽  
Total Chloride ◽  
Flame Ionization ◽  
Sample Extract ◽  
Chromatographic Procedure ◽  
Liquid Chromatographic

Abstract A simple and rapid gas-liquid chromatographic method, using flame ionization detection and a column packed with OV-17/QF-1 on Gas-Chrom Q, is described. Chlorpyriphos is extracted from the formulation with chloroform, and dieldrin is added as an internal standard. The sample extract is injected into a gas chromatograph, and peak height ratios are used for quantitative measurement. Applicacation of the method to commercial samples gives good precision. The gas chromatographic procedure is far superior to the total chloride method for the determination of chlorpyriphos and yields values in close agreement to those obtained by infrared and colorimetric methods.

Gas-Liquid Chromatographic Determination of p-Chloroacetanilide in Acetaminophen

1978 ◽  
Vol 61 (1) ◽  
pp. 68-71
Author(s):  
Dorothy K Wyatt ◽  
Lee T Grady
Keyword(s):  
Liquid Chromatography ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Gas Liquid Chromatography ◽  
Flame Ionization ◽  
Glass Column ◽  
Retention Characteristics ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract Gas-liquid chromatography (GLC) coupled with column chromatography was used to accurately determine as little as 25 ppm p-chloroacetanilide in acetaminophen. p-Chloroacetanilide was eluted from a pH 8 phosphate-buffered diatomite partition column by using purified tetrachloroethylene (acetaminophen was retained). This solution was concentrated, internal standard (docosane) was added, and p-chloroacetanilide was determined by using a 0.9 m × 2 mm glass column packed with 3% Poly A 103 on Supelcoport and a flame ionization detector with electronic integration. Standard curves were linear for 10–100 ppm p-chloroacetanilide. Various chromatographic materials were investigated for optimal retention characteristics. High pressure liquid chromatography (HPLC) was also evaluated as an alternative; however, lack of reproducibility of the HPLC column favored the GLC procedure.

Gas-Liquid Chromatographic Determination of Phenothiazine in Medicated Feeds

1973 ◽  
Vol 56 (1) ◽  
pp. 174-176
Author(s):  
Billy M Colvin ◽  
Albert E Prudom ◽  
Larry L Whitlock ◽  
Alan R Hanks
Keyword(s):  
Internal Standard ◽  
Chromatographic Determination ◽  
Peak Height ◽  
Good Precision ◽  
Gas Chromatograph ◽  
Aoac Method ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Medicated Feeds

Abstract A simple and rapid method is described for the determination of phenothiazine in feeds. Phenothiazine is extracted with chloroform containing chlorobenzilate as an internal standard. The extract is injected into a gas chromatograph and peak height ratios are used for quantitation. The analysis of commercial samples shows that the method compares well with the more commonly employed colorimetric AOAC method, and good precision, with recoveries ranging from 96.0 to 99.9%, is obtained in the analysis of prepared samples.

Gas-Liquid Chromatographic Determination of Paraldehyde in Paraldehyde Elixir

1972 ◽  
Vol 55 (1) ◽  
pp. 166-169
Author(s):  
William T Lampkin
Keyword(s):  
Collaborative Study ◽  
Internal Standard ◽  
Pharmaceutical Preparations ◽  
Standard Technique ◽  
Chromatographic Determination ◽  
Flame Ionization ◽  
Glass Column ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A collaborative study was conducted on a GLC method for determining paraldehyde in pharmaceutical preparations of paraldehyde elixirs. Eleven collaborating laboratories analyzed 2 unknown paraldehyde solutions and a solution of known paraldehyde concentration. Recoveries of 15–25% paraldehyde solutions averaged 98.5% with a coefficient of variation of about 2%. The method consists of diluting a sample aliquot to a definite volume and determining the paraldehyde content by GLC, using a flame ionization detector and a 6’ × 4 mm coiled glass column packed with 80–100 mesh Diatoport S coated with 2% HIEFF-8BP (cyclohexane dimethanol succinate) plus 20% Carbowax 20M. The internal standard technique was used for calculation. It is recommended that the method be adopted as official first action.

Gas-Liquid Chromatographic Determination of Disulfoton in Formulations: Collaborative Study

1980 ◽  
Vol 63 (4) ◽  
pp. 869-872
Author(s):  
Thomas L Jensen ◽  
◽  
J B Audino ◽  
R Bishop ◽  
L Chenery ◽  
...  
Keyword(s):  
Collaborative Study ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Peak Height ◽  
Flame Ionization ◽  
Average Coefficient ◽  
Liquid Chromatographic Determination ◽  
Gasliquid Chromatography ◽  
Liquid Chromatographic

Abstract A rapid method is described for the determination of disulfoton (0,0-diethyl S-[2-(ethylthio)-ethyl] phosphorodithioate) in formulations by gasliquid chromatography (GLC). Samples are dissolved in acetone, and, after an internal standard is added, the samples are diluted to volume with solvent. They are then injected into a gas chromatograph equipped with a flame ionization detector and quantitated by peak height or area measurements. Fourteen collaborators made duplicate determinations on 4 samples including the technical product, a liquid, and 2 granular formulations. The average coefficient of variation was 0.847% for the liquid samples and 1.90% for the granules. The 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.

Gas-Liquid Chromatographic Determination of Pyridazinones in Technical Products and Formulations

1978 ◽  
Vol 61 (1) ◽  
pp. 161-163
Author(s):  
Giuseppe Cellerino ◽  
Mariarosa Re
Keyword(s):  
Internal Standard ◽  
Standard Technique ◽  
Chromatographic Determination ◽  
Gas Liquid Chromatography ◽  
Flame Ionization ◽  
Selective Detector ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Technical Products

Abstract Simultaneous determination of the active ingredient and of by-products in technical and formulated pyridazinones was rapidly performed by gas-liquid chromatography with complete resolution of all compounds. Quantitative determination by the internal standard technique is accurate and precise. The lower limit of detectability is 8 × 10–12 g/sec with a flame ionization detector and 1 × 10–12 g/sec with a nitrogen-phosphorus selective detector operating in the nitrogen mode.

Reverse Phase High Performance Liquid Chromatographic Determination of Phenprocoumon in Tablets

1982 ◽  
Vol 65 (3) ◽  
pp. 753-756
Author(s):  
Walter F Schmidt
Keyword(s):  
High Performance ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
High Performance Liquid Chromatographic ◽  
Reverse Phase ◽  
Assay Procedure ◽  
Chromatographic Procedure ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A high performance liquid chromatographic procedure has been developed for the assay of phenprocoumon in tablets. In comparison to the present official USP assay procedure, it is equivalent in precision and accuracy and is faster and more specific. A mobile phase consisting of a 1% solution of acetic acid in acetonitrile-water (4 + 3) separates phenprocoumon from warfarin internal standard on a 6 μm octadecylsilane (ODS) column with UV detection at 311 nm. The method enables the concurrent determination of phenprocoumon and possible contaminants such as salicylic acid.

Gas-Liquid Chromatographic Determination of Isosorbide Dinitrate in Tablets

1977 ◽  
Vol 60 (6) ◽  
pp. 1341-1344
Author(s):  
David G Prue ◽  
Raymond N Johnson ◽  
Boen T Kho
Keyword(s):  
Isosorbide Dinitrate ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Raw Material ◽  
Phase System ◽  
Flame Ionization ◽  
Coefficients Of Variation ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A gas-liquid chromatographic (GLC) method is described for determining isosorbide dinitrate (ISDN) in tablets. ISDN is extracted from tablet excipients by a 2-phase system composed of water-ethyl ether, and detected and quantitated with a flame ionization detector after separation from the internal standard (glyceryl tributyrate) on a 3% OV-210 column. Ten replicate assays on 2 different batches of tablets, each containing 5 mg ISDN, gave coefficients of variation of 1.16 and 1.48%, respectively. Comparison of results obtained for tablets containing 5, 10, and 40 mg ISDN, and for diluted isosorbide dinitrate raw material containing 25% ISDN, showed good correlation among the GLC, USP colorimetric, and USP polarographic procedures. Assay of synthetic mixtures containing ISDN, isosorbide-2-mononitrate, and isosorbide-5-mononitrate demonstrated that the GLC procedure is specific for ISDN, whereas the USP polarographic procedure is subject to interference from the mononitrates.

Gas-Liquid Chromatographic Determination of Pentachloronitrobenzene in Pesticide Formulations

1976 ◽  
Vol 59 (3) ◽  
pp. 708-710
Author(s):  
Alan R Hanks ◽  
Christine W Cramer
Keyword(s):  
Chromatographic Method ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Peak Height ◽  
Liquid Chromatographic Method ◽  
Pesticide Formulations ◽  
Liquid Chromatographic Determination ◽  
Standard Solution ◽  
Liquid Chromatographic

Abstract A gas-liquid chromatographic method has been developed to determine pentachloronitrobenzene (PCNB) in pesticide formulations including dusts, powders, granules, liquids, and fertilizers. Captan, disulfoton, and Terrazole do not interfere. Samples are extracted with chloroform, and an aliquot is mixed with an equal volume of internal standard solution containing o-terphenyl. PCNB is chromatographed on a 5% SE-30 column and quantitated by peak height ratios. The method has been subjected to a ruggedness test which indicates little sensitivity to changes in extraction and chromatographic conditions.

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