Gas-Liquid Chromatographic Determination of Diethylstilbestrol Monomethyl Ether in Diethylstilbestrol

1974 ◽  
Vol 57 (1) ◽  
pp. 79-81
Author(s):  
Frank E Gainer ◽  
William J Chiasson
Keyword(s):  
Sodium Hydroxide ◽  
Chloroform Solution ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Monomethyl Ether ◽  
Detector Response ◽  
Internal Standard Peak ◽  
Gas Chromatographic Method ◽  
Liquid Chromatographic

Abstract A gas chromatographic method is described for the determination of the monomethyl ether of diethylstilbestrol (MME) in diethylstilbestrol (DES). A 1 g sample of DES is dissolved in an aqueous solution of 0.5N sodium hydroxide and extracted with a chloroform solution containing benefin, the internal standard. The chloroform solution is back-extracted with sodium hydroxide, and an aliquot is chromatographed after silylation. The MME peaks (cis and trans') are measured relative to the internal standard peak. The method was tested for accuracy within the 120—2000 ppm range, and a linear plot of detector response vs. concentration was obtained. The method is also suitable for the determination of diethylstilbestrol dimethyl ether (DME) if present with MME in a DES sample.

Gas Chromatographic Determination of Diethylstilbestrol Dimethyl Ether in Diethylstilbestrol

1972 ◽  
Vol 55 (1) ◽  
pp. 185-186
Author(s):  
F E Gainer ◽  
W J Chiasson
Keyword(s):  
Aqueous Solution ◽  
Dimethyl Ether ◽  
Chloroform Solution ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Detector Response ◽  
Chloroform Layer ◽  
Internal Standard Peak ◽  
Linear Plot

Abstract A GLC method is described for the determination of the dimethyl ether of diethylstilbestrol (DME) in diethylstilbestrol (DES). A 1 g sample of DES is dissolved in an aqueous solution of 0.5N NaOH and then extracted with a chloroform solution containing benefin, the internal standard. An aliquot of the chloroform layer is chromatographed and the DME peak is measured relative to the internal standard peak. The method was tested for accuracy within the 11–110 ppm range and a linear plot of detector response vs. concentration was obtained.

Improved liquid-chromatographic determination of mexiletine, an antiarrhythmic drug, in plasma.

1984 ◽  
Vol 30 (2) ◽  
pp. 319-322 ◽  
Author(s):  
W Mastropaolo ◽  
D R Holmes ◽  
M J Osborn ◽  
J Rooke ◽  
T P Moyer
Keyword(s):  
Methylene Chloride ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Peak Height ◽  
Reversed Phase ◽  
Internal Standard Peak ◽  
Chromatographic Procedure ◽  
Liquid Chromatographic

Abstract In this improved reversed-phase liquid-chromatographic procedure for determination of mexiletine in plasma, mexiletine and an internal standard, chlorodisopyramide, are extracted with methylene chloride from 0.5 mL of serum or plasma; the extract is then concentrated and injected onto a C18 chromatographic column. Mexiletine in the column effluent is detected by monitoring absorbance at 210 nm. It is quantified by use of mexiletine-internal standard peak-height ratios. The relation between this ratio and mexiletine concentration is linear from 0.1 to 5.0 mg/L. The lower limit of detection is about 50 micrograms/L. At a mexiletine concentration of 2.0 mg/L in serum, intrarun precision (CV) is 2.9% and inter-run precision is 5.9%; at 0.5 mg/L, these CVs are 5.7% and 9.6%, respectively. Analytical recovery of added mexiletine in serum is 68-88%. Therapeutic concentrations of some commonly administered drugs in patients' specimens did not interfere. In serum from 38 patients receiving mexiletine for cardiac arrhythmia, concentrations measured by this method correlated with therapeutic efficacy.

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 Diethylstilbestrol at Low Levels in Mixed Feeds

1976 ◽  
Vol 59 (4) ◽  
pp. 821-824
Author(s):  
Richard G Einig
Keyword(s):  
Sodium Hydroxide ◽  
Chloroform Solution ◽  
Chromatographic Determination ◽  
Carbonate Buffer ◽  
Liquid Chromatographic Method ◽  
Glass Column ◽  
Liquid Chromatographic Determination ◽  
Mixed Feeds ◽  
Liquid Chromatographic

Abstract A gag-liquid chromatographic method for the determination of diethylstilbestrol (DES) at 2 ppb in mixed feeds and ingredients is presented. The DES is extracted into ethanol, the solvent is evaporated, and the residue is redissolved in chloroform. The extract is purified by washing the chloroform solution with carbonate buffer and transferring the DES to sodium hydroxide. The sodium hydroxide is washed with chloroform, the pH is adjusted to 10.3, and the DES is transferred to chloroform. The extract is derivatized with heptafiuorobutyric anhydride, chromatographed on an SE-30 glass column, and measured with a 3H electron capture detector. The method has been used for routine testing of a wide variety of feeds and ingredients.

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.

scholarly journals High-performance liquid chromatographic determination of famotidine in human plasma using solid-phase column extraction

2003 ◽  
Vol 68 (11) ◽  
pp. 883-892 ◽  
Author(s):  
Dragica Zendelovska ◽  
Trajce Stafilov
Keyword(s):  
Human Plasma ◽  
High Performance ◽  
Solid Phase ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
High Performance Liquid Chromatographic ◽  
Water Ph ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

A rapid, specific and sensitive high-performance liquid chromatographic method for the determination of famotidine in human plasma has been developed. Famotidine and the internal standard were chromatographically separated from plasma components using a Lichrocart Lichrospher 60 RP select B cartridge for solid-phase separation with a mobile phase composed of 0.1 % (v/v) triethylamine in water (pH 3) and acetonitrile (92:8, v/v). UV detection was set at 270 nm. The calibration curve was linear in the concentration range of 10.0 ? 350.0 ng mL-1. The method was implemented to monitor the famotidine levels in patient samples.

Improved liquid-chromatographic determination of haloperidol in plasma.

1984 ◽  
Vol 30 (7) ◽  
pp. 1228-1230 ◽  
Author(s):  
A K Dhar ◽  
H Kutt
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Room Temperature ◽  
Internal Standard ◽  
Isoamyl Alcohol ◽  
Chromatographic Determination ◽  
Reversed Phase ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract This method for determination of haloperidol in plasma is based on "high-performance" isocratic liquid chromatography with the use of a C8 bonded reversed-phase column at room temperature. Haloperidol and the internal standard (chloro-substituted analog) are extracted from alkalinized plasma into isoamyl alcohol/heptane (1.5/98.5 by vol) and back-extracted into dilute H2SO4. The aqueous phase is directly injected onto the column. The mobile phase is a 30/45/25 (by vol) mixture of phosphate buffer (16.5 mmol/L, pH 7.0), acetonitrile, and methanol. Unlike other liquid-chromatographic procedures for haloperidol, commonly used psychotropic drugs do not interfere. Analysis can be completed within an hour. The procedure is extremely sensitive (1.0 microgram/L) and is well reproducible (CV 5.6% for a 2.5 micrograms/L concentration in plasma).

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.

Liquid Chromatographic Determination of Methiocarb in Technical and Formulated Products: Collaborative Study

1984 ◽  
Vol 67 (3) ◽  
pp. 492-493
Author(s):  
Stephen C Slahck ◽  
◽  
A A Carlstrom ◽  
L T Chenery ◽  
N D Ellis ◽  
...  
Keyword(s):  
Coefficient Of Variation ◽  
Collaborative Study ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Reverse Phase ◽  
Reverse Phase Chromatography ◽  
Wettable Powder ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract An LC method for the determination of methiocarb in methiocarb technical and formulated products has been subjected to a collaborative study with 9 participating collaborators. Formulations are extracted with acetonitrile and analyzed by reverse phase chromatography, with acetophenone as an internal standard. Collaborators were furnished samples of technical, 75% wettable powder, 75% seed treater, 75% concentrate, and 50% hopper box treater. Coefficient of variation values obtained on the 5 samples were 0.71, 0.83, 0.62, 1.57, and 0.82%, respectively. The method has been adopted official first action.

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