Determination of Vitamins D2 and D3 in Pharmaceuticals by Gas-Liquid Chromatography

1968 ◽  
Vol 51 (4) ◽  
pp. 839-840
Author(s):  
T K Murray ◽  
P Erdody ◽  
T Panalaks
Keyword(s):  
Vitamin D ◽  
Liquid Chromatography ◽  
Vitamin A ◽  
Coefficient Of Variation ◽  
Internal Standard ◽  
Antimony Trichloride ◽  
The Other ◽  
Gas Liquid Chromatography ◽  
Partition Chromatography

Abstract A method is described for determining vitamin D in multivitamin preparations; in the method, vitamins D2 and D3 are isomerized with antimony trichloride and separated by GLC. Vitamins D,2 and D3 are differentiated and measured separately and one vitamin may be used as an internal standard for the other. Vitamin A is largely removed by partition chromatography but can be tolerated in the final dilution in a ratio of 1:1 with vitamin D. When the method was used for the assay of multivitamin preparations, the coefficient of variation was 3.2%.

Separation of Vitamins D2 and D3 as Isotachysterols D2 and D3 by Gas-Liquid Chromatography

1968 ◽  
Vol 51 (4) ◽  
pp. 834-838
Author(s):  
A J Sheppard ◽  
Denis E Lacroix ◽  
A R Prosser
Keyword(s):  
Liquid Chromatography ◽  
Quantitative Determination ◽  
Infrared Absorption ◽  
Quantitative Measurement ◽  
Acetyl Chloride ◽  
Internal Standard ◽  
The Other ◽  
Gas Liquid Chromatography ◽  
Absorption Data

Abstract A method for the quantitative determination of 0.5—20 μg vitamins D2 and D3 by gas-liquid chromatography is described. Vitamins D2 and D3 are completely isomerized to their respective isotachysterol isomers by acetyl chloride as demonstrated by ultraviolet and infrared absorption data. Dihydrotachysterol D2, isotachysterol D2, and isotachysterol D3 are completely resolved with a 3% JXR on 100-120 mesh Gas Chrom Q column packing. Calibration studies show that each compound exhibited a characteristic dose-response plot. Therefore, one isomer cannot be used as a direct internal standard for the quantitative measurement of the other isomer.

DETERMINATION OF PLASMA OESTRIOL IN NORMAL PREGNANCY AND LABOUR USING GAS-LIQUID CHROMATOGRAPHY

1971 ◽  
Vol 51 (3) ◽  
pp. 447-454 ◽  
Author(s):  
W. COOPER ◽  
M. G. COYLE ◽  
J. A. MILLS
Keyword(s):  
Gas Chromatography ◽  
Liquid Chromatography ◽  
Quantitative Determination ◽  
Internal Standard ◽  
Normal Pregnancy ◽  
Gas Liquid Chromatography ◽  
Chemical Purification ◽  
Peripheral Plasma ◽  
Pregnancy And Delivery

SUMMARY A method is described for estimating oestriol in 2–10 ml samples of human pregnancy peripheral plasma. It incorporates acid hydrolysis, chemical purification, methylation, chromatography on alumina columns, formation of a derivative and quantitative determination by gas chromatography. A radioactive internal standard was added to correct for procedural losses. Plasma oestriol determinations in five normal patients throughout pregnancy and delivery are reported.

Rapid Method for Quantitative Determination of Propoxyphene in Serum by Gas-Liquid Chromatography

1973 ◽  
Vol 19 (5) ◽  
pp. 492-495 ◽  
Author(s):  
M A Evenson ◽  
Susan Koellner
Keyword(s):  
Liquid Chromatography ◽  
Quantitative Determination ◽  
Rapid Method ◽  
Coefficient Of Variation ◽  
Therapeutic Dose ◽  
Gas Liquid Chromatography ◽  
Healthy Controls ◽  
Serum Pool ◽  
Sedative Drugs

Abstract Rapid, accurate, and precise gas-chromatographic methods are reported for measurement of propoxyphene ("Darvon") in serum. A sample of 5 ml of serum is required for quantitation in blood after a therapeutic dose of 130-195 mg of propoxyphene; in cases of overdose of propoxyphene, only 1 ml of serum is required in a "toxic method" variation. Neither serum from healthy controls or from hospitalized patients contains interfering substances. Several commonly used analgesic and sedative drugs, added to a serum pool, also did not interfere. Day-to-day precision of the therapeutic method, as measured by the coefficient of variation (CV), is 7%; the CV for the method as applied to overdose cases is less than 3%. Propoxyphene added to serum could be about 86% accounted for analytically.

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.

Gas Chromatographic Methods for Determination of γ-BHC in Technical Emulsifiable Concentrates and Water-Dispersible Powder Formulations and in Lindane Shampoo and Lotion: Collaborative Study

1984 ◽  
Vol 67 (4) ◽  
pp. 834-837
Author(s):  
James W Miles ◽  
Dwight L Mount ◽  
◽  
T J Beckmann ◽  
S K Carrigan ◽  
...  
Keyword(s):  
Coefficient Of Variation ◽  
Collaborative Study ◽  
Internal Standard ◽  
The Other ◽  
Water Dispersible ◽  
Coefficients Of Variation ◽  
Aoac Method ◽  
Liquid Chromatographic ◽  
Gas Chromatographic Separation

Abstract Although the gas chromatographic separation of the isomers of BHC was demonstrated two decades ago, the present AOAC method of analysis of BHC for gamma-isomer (lindane) content is based on a separation carried out on a liquid chromatographic partition column. A method of analysis has been developed that uses an OV-210 column for separation of the gamma-isomer from the other isomers and impurities in technical BHC. Di-n-propyl phthalate was chosen as an internal standard. The same system allows quantitation of lindane in lotion and shampoo after these products are extracted with ethyl acetate-isooctane (1 + 4). The analytical methods were subjected to a collaborative trial with 10 laboratories. The coefficient of variation for technical BHC was 2.83%. For the water-dispersible powder and emulsifiable concentrate, the coefficients of variation were 2.89% and 4.62%, respectively. Coefficients of variation for 1% lindane lotion and shampoo were 4.36% and 11.92%, respectively. The method has been adopted official first action.

Gas-Liquid Chromatographic Determination of β-Asarone in Wines and Flavors

1976 ◽  
Vol 59 (3) ◽  
pp. 675-677
Author(s):  
Randolph H Dyer ◽  
Glenn E Martin ◽  
Peter C Buscemi
Keyword(s):  
Liquid Chromatography ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Gas Liquid Chromatography ◽  
Ethyl Palmitate ◽  
Ultraviolet Spectra ◽  
Liquid Chromatographic Determination ◽  
Mass Spectrometery ◽  
Liquid Chromatographic

Abstract Wine samples containing β-asarone (cis-2,4,5-trimethoxy-1-propenylbenzene) are distilled; β-asarone is extracted by hexane and then quantitatively determined by gas-liquid chromatography (GLC), using ethyl palmitate as the internal standard. The GLC procedure is rapid and yields precise and accurate results. Mass spectrometery confirmed the identity of the GLC peak as β-asarone. The ultraviolet spectra of β-asarone and its isomer were also determined.

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.

Determination of Siduron in Fertilizers by Flame Ionization Gas-Liquid Chromatography

1974 ◽  
Vol 57 (1) ◽  
pp. 60-61
Author(s):  
Daniel B Ealy ◽  
Robert R Gorman ◽  
Francis R Kaiser ◽  
Robert E Scroggs
Keyword(s):  
Liquid Chromatography ◽  
Internal Standard ◽  
Gas Liquid Chromatography ◽  
Flame Ionization ◽  
Magnetic Stirrer ◽  
Hydrogen Flame ◽  
Mode Of Detection

Abstract Siduron is formulated with fertilizers at about 2.4%. The herbicide is extracted with CHC13, using a magnetic stirrer, p,p'-methoxychlor is added as an internal standard, and the relative GLC peak heights are determined. The GLC column is 3% JXR on Gas-Chrom Q, and the mode of detection is hydrogen flame ionization.

Determination of Amitraz in Cattle Dipping Baths and Sprays

1978 ◽  
Vol 61 (6) ◽  
pp. 1516-1518
Author(s):  
Michael V Machin ◽  
Kerryn W Mcdougall
Keyword(s):  
Liquid Chromatography ◽  
Petroleum Ether ◽  
Coefficient Of Variation ◽  
Gas Liquid Chromatography ◽  
Chromatographic Methods ◽  
Coefficients Of Variation

Abstract Infrared (IR) and gas chromatographic methods have been developed for determining the acaricide amitraz (N-(2,4-dimethylphenyl)-N - [[(2,4- dimethylphenyl)imino]methyl] - N - methanimidamide) in cattle dip solutions. Extraction with petroleum ether, followed by IR and gas-liquid chromatography (GLC) gave coefficients of variation of 3.4 and 3.6%, respectively, for 0.010-0.035% amitraz. Dilution of the dip sample with acetone and determination by GLC gave a coefficient of variation of 3.6% in the same range. Recovery of amitraz from fortified dip samples was 97–100%.

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