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

1981 ◽  
Vol 64 (6) ◽  
pp. 1315-1318
Author(s):  
Peter D Bland ◽  
◽  
J Bagness ◽  
W Black ◽  
L Brown ◽  
...  
Keyword(s):  
Collaborative Study ◽  
Chloroform Solution ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Gas Liquid Chromatography ◽  
Technical Product ◽  
Flame Ionization ◽  
Peak Areas ◽  
Liquid Chromatographic

Abstract A method is described for the determination of pirimicarb (2-(dimethylamino)-5,6-dimethyl-4-pyrimidinyl dimethylcarbamate) in formulated products by gas-liquid chromatography (GLC). Samples are dissolved in a chloroform solution of an internal standard and injected into a gas chromatograph equipped with a flame ionization detector. Quantitative data are obtained by comparing peak areas of the compound and internal standard with those obtained by injecting a standard solution. Eleven collaborators made replicate determinations on 6 samples including a technical product, a granular product, and 4 powder products. The average coefficient of variation was 1.14% for the technical product, 1.82% for the granular product, and 0.73% for the powder products.

Capillary Gas Chromatographic Determination Of Cypermethrin In Formulations: Collaborative Study

1985 ◽  
Vol 68 (3) ◽  
pp. 592-595
Author(s):  
Peter D Bland
Keyword(s):  
Active Ingredient ◽  
Collaborative Study ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Fused Silica ◽  
Flame Ionization ◽  
Wettable Powder ◽  
Peak Areas ◽  
Liquid Concentrate

Abstract A method is described for the determination of cypermethrin, 3-(2,2- dichloroethenyl)-2,2-dimethyl-cyclopropanecarboxylate cyano-(3- phenoxyphenyl)methyl ester, in technical and formulated material by capillary gas chromatography (CGC). Samples of technical or formulated material are dissolved in CH2Cl2 containing dicyclohexyl phthalate as internal standard. The solution is injected into a gas chromatograph fitted with a flame ionization detector and capillary column of 25 m x 0.32 mm fused silica with a thick film OV-1 phase at 240°C. Injection is made into a heated injection port fitted with an antidiscrimination device in a split mode. Peak areas obtained at retention times of the internal standard and active ingredient are measured with an integrator. The quantity of cypermethrin is determined by comparing the internal standard and active ingredient peak areas with those obtained from a calibration solution containing known amounts of internal standard and pure active ingredient. Five samples were chosen for collaborative study: technical cypermethrin, 70% liquid concentrate, 3 lb/US gal. emulsifiable, 3 ib/US gal. oil concentrate, and 40% wettable powder. Twelve collaborators carried out replicate determinations on each sample on separate days. Coefficients of variation between laboratories (CVX) were 2.13 for the technical, 2.94 for the emulsifiable concentrate, 3.51 for the liquid concentrate, 2.66 for the wettable powder, and 2.29 for the oil concentrate. The method was adopted 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.

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.

Collaborative Study of Gas-Liquid Chromatographic Determination of Methaqualone in Pharmaceutical and Clandestine Preparations

1977 ◽  
Vol 60 (4) ◽  
pp. 935-939 ◽  
Author(s):  
Harold F Hanel
Keyword(s):  
Liquid Chromatography ◽  
Quantitative Determination ◽  
Collaborative Study ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Gas Liquid Chromatography ◽  
Coefficients Of Variation ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract Eight laboratories collaboratively studied a procedure for the quantitative determination of methaqualone. HCl in pharmaceutical and clandestine preparations. Methaqualone is extracted from an aqueous bicarbonate solution into chloroform and quantitated by gas-liquid chromatography on a 3% OV-1 column. Tetraphenylethylene is used as an internal standard. Two commercial preparations and 4 sample mixtures prepared by the author were studied. Recoveries for the 4 prepared samples ranged from 100.0 to 102.6%, and the coefficients of variation ranged from 1.58 to 4.15% for the 6 samples studied. The method has been adopted as official first action.

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.

Collaborative Study of the Gas-Liquid Chromatographic Determination of Malathion in Formulations and Technical Materials

1979 ◽  
Vol 62 (2) ◽  
pp. 292-296
Author(s):  
Richard S Wayne
Keyword(s):  
Collaborative Study ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Technical Grade ◽  
Flame Ionization ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Action Methods

Abstract A gas-liquid chromatographic method was studied collaboratively for determining malathion in wettable powders, an emulsifiable concentrate, a dust, and the technical grade product. Flame ionization detection, m-diphenoxybenzene as the internal standard, and a column containing 5% SP-2401 or OV-210 on 100-120 mesh Gas-Chrom Q or Supelcoport were used for the determination. Agreement between replicates in individual laboratories was excellent. Agreement between laboratories was satisfactory. The method offers improved specificity and ease of operation when compared to the official first action methods. The method has been 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 Terbuthylazine Technical and Its Formulations: Collaborative Study

1981 ◽  
Vol 64 (4) ◽  
pp. 825-828
Author(s):  
Juerg Meier ◽  
Klaus Nowak ◽  
Rolf Suter ◽  
Andrea Tomann ◽  
Hans P Bosshardt ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Collaborative Study ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Gas Liquid Chromatography ◽  
Wettable Powder ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract Terbuthylazine technical and its 80% wettable powder were analyzed in a CIPAC collaborative study. The content and the identity were determined by gas-liquid chromatography on a column of 3% Carbowax K20M on Gas-Chrom Q, using di-n-pentylphthalate as the internal standard. Results obtained from 27 government, university, and industrial collaborators showed within-laboratory repeatability of 1.3% for the technical and 1.0% for the wettable powder. Reproducibility was 2.1% for both samples. The method has been adopted official first action

Liquid Chromatographic Determination of Diazepam in Tablets: Collaborative Study

1985 ◽  
Vol 68 (3) ◽  
pp. 545-546
Author(s):  
Michael Tsougros
Keyword(s):  
Collaborative Study ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Reverse Phase ◽  
Photometric Detection ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic Determination ◽  
The Mean ◽  
Liquid Chromatographic

Abstract A stability indicating liquid chromatographic method for the determination of diazepam in tablets was collaboratively studied by 6 laboratories. The method uses a Cig reverse phase column, a methanolwater mobile phase, p-tolualdehyde as the internal standard, and photometric detection at 254 nm. The collaborators were supplied with a synthetic tablet powder and 3 commercial tablet samples. The mean recovery of diazepam from the synthetic tablet powder was 100.2%. For all samples analyzed, the coefficient of variation was < 1.5%. The method has been adopted official first action.

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