Gas-Liquid Chromatographic Determination of Oxydemeton-Methyl in Commercial Formulations

1978 ◽  
Vol 61 (3) ◽  
pp. 500-503
Author(s):  
Leonard R Schronk ◽  
Billy M Colvin ◽  
Alan R Hanks
Keyword(s):  
Rapid Determination ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Peak Height ◽  
Detector Response ◽  
Gel Chromatography ◽  
Gas Liquid Chromatography ◽  
Flame Ionization ◽  
Silica Gel Chromatography

Abstract Flame ionization gas-liquid chromatography (GLC) with a 10% DC-200 on 80-100 mesh Gas-Chrom Q column is used for the rapid determination of oxydemeton-methyl in commercial formulations. The detector response is linear for 1.0–10.0 μg oxydemeton-methyl, with a sensitivity of 4 ng. The column was stabilized before analysis by injection of a lecithin solution. Samples were diluted with chloroform and injected; peak height ratios were used for quantitation with fluoranthrene as the internal standard. Carbaryl was removed from mixed formulations by silica gel chromatography, oxydemeton- methyl was eluted with methanolchloroform (2+98), and the eluate was collected for infrared (IR) and GLC analyses. Methoxychlor and Karathane were removed by chromatography on Florisil before IR analysis. GLC results compare favorably with those for IR, with recoveries ranging from 98.44 to 102.88% for spiked formulations.

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.

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.

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 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 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.

Flame ionization detector response to coeluting hydrocarbons and carbon disulphide and its application to the determination of the sum of C6-C11 alkanes and cycloalkanes in air

1983 ◽  
Vol 48 (3) ◽  
pp. 722-734
Author(s):  
Martin Koval
Keyword(s):  
Carbon Disulphide ◽  
Internal Standard ◽  
Calibration Procedure ◽  
Detector Response ◽  
Column Temperature ◽  
Flame Ionization ◽  
Other Substances ◽  
Flame Ionisation Detector ◽  
Ionisation Detector

The flame ionisation detector response to C6-C11 aliphatic hydrocarbon solutions in carbon disulphide in the concentration range between 1.3-9.5 mg ml-1 retained lineary despite the excess of solvent entering the detector simultaneously with the analyte. Pure carbon disulphide exhibited a small positive detector response which did not interfere in calibration procedure and which, under certain GC conditions, inverted to negative values. This response was not proportional to the injected volume and was strongly influenced by the column temperature and/or bleed. On the basis of these findings, a method compatible with the widely used charcoal tube carbon disulphide desorption procedure was developed and evaluated. It consists of static desorption of the sum of aliphatic alkanes and cycloalkanes from the activated charcoal after which an internal standard is added to the supernatant eluate. The resulting carbon disulphide solution is analysed on a highly polar stationary phase 1,2,3-tris(2-cyanoethoxy)propane where the solvent and the analyte coelute in a single peak, the height of which is practically proportional to the sum of alkanes and cycloalkanes present. This also makes determinations of other substances present in the sample more simple. The field test of the proposed method yielded values comparable in precision and accuracy with a control infrared spectrophotometric method.

Optimized liquid-chromatographic determination of metronidazole and its metabolites in plasma.

1984 ◽  
Vol 30 (5) ◽  
pp. 784-787 ◽  
Author(s):  
R A Gibson ◽  
L Lattanzio ◽  
H McGee
Keyword(s):  
Rapid Determination ◽  
Chromatographic Determination ◽  
Reversed Phase ◽  
Detector Response ◽  
High Pressure Liquid Chromatographic ◽  
Liquid Chromatographic Method ◽  
Wide Range ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract Metronidazole and its known metabolites in plasma can be rapidly separated by a "high-pressure" liquid-chromatographic method that can also be adapted for rapid determination of tinidazole. Samples deproteinized with trichloroacetic acid (50 g/L final concentration) undergo isocratic separation on a reversed-phase C18 column eluted with an 8/92 (by vol) mixture of acetonitrile/KH2PO4 (5 mmol/L, pH 3.0). The method is sensitive, reliably detecting as little as 25 micrograms of metronidazole and (or) its metabolites per milliliter of plasma. The detector response varied linearly with concentration for all compounds tested over a wide range (25-500 micrograms/L). Within-day and between-day variation was generally less than 2.5% for all concentrations of all compounds tested. Various other antibiotics tested did not interfere.

Gas-chromatographic determination of cholesterol sulfate in plasma and erythrocytes, for the diagnosis of recessive X-linked ichthyosis.

1983 ◽  
Vol 29 (7) ◽  
pp. 1404-1407 ◽  
Author(s):  
F A Muskiet ◽  
G Jansen ◽  
B G Wolthers ◽  
A Marinkovic-Ilsen ◽  
P C van Voorst Vader
Keyword(s):  
Internal Standard ◽  
Dehydroepiandrosterone Sulfate ◽  
Chromatographic Determination ◽  
Anion Exchange Chromatography ◽  
Exchange Chromatography ◽  
Single Step ◽  
Flame Ionization Detection ◽  
Cholesterol Sulfate ◽  
Flame Ionization

Abstract We describe a rapid method for determining cholesterol sulfate in plasma and erythrocytes. After its single-step isolation by means of anion-exchange chromatography cholesterol sulfate is hydrolyzed, trimethylsilylated, and determined by gas chromatography with flame ionization detection. 5 beta-Cholestan-3 alpha-ol sulfate is used as internal standard. The method enables simultaneous determination of dehydroepiandrosterone sulfate in plasma. We applied it for the diagnosis of seven patients with recessive X-linked ichthyosis. Concentrations are given for plasma and erythrocytes from four unaffected relatives of patients with X-linked ichthyosis, a patient with placental sulfatase deficiency, two patients with other types of ichthyoses, and 20 controls. The method may also be of use for the rapid isolation of other organic sulfates from biological material, as illustrated by a comparison of gas chromatograms of urine from a normal pregnant woman and that from a patient with placental sulfatase deficiency.

Determination of Phenothiazine and Several of its Derivatives by Gas-Liquid Chromatography

1966 ◽  
Vol 49 (4) ◽  
pp. 857-859
Author(s):  
C L Bramlett
Keyword(s):  
Liquid Chromatography ◽  
Internal Standard ◽  
Flame Ionization Detector ◽  
Gas Liquid Chromatography ◽  
Chromatographic Technique ◽  
Ionization Detector ◽  
Flame Ionization ◽  
Hydrogen Flame

Abstract Phenothiazine, promethazine.HCl, chlorpromazine. HCl, promazine.HCl, and levomepromazine. HCl were chromatographed satisfactorily on a column containing 5% Apiezon L coated on Anakrom ABS, 100/110 mesh, using a hydrogen-flame ionization detector. This gas chromatographic technique is rapid and more specific than existing official methods. The use of an internal standard to improve precision will be investigated.

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