Liquid Chromatographic Determination of Strychnine in Stomach Contents

1985 ◽  
Vol 68 (6) ◽  
pp. 1131-1133
Author(s):  
Jacobus J L Hoogenboom ◽  
Colin G Rammell
Keyword(s):  
Phosphoric Acid ◽  
Stomach Contents ◽  
Chromatographic Determination ◽  
Chloroform Extract ◽  
Acid Extract ◽  
Reverse Phase ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Phase Column

Abstract A chloroform extract of stomach contents at basic pH is concentrated and then extracted with 0.1M phosphoric acid. The acid extract is chromatographed on a 10 cm reverse phase column, using 0.005M phosphate buffer (pH 3.0)-acetonitrile-tetrahydrofuran (750 + 135 + 115) containing 0.01M octanesulfonic acid at a flow rate of 1.0 raL/ min for elution. Strychnine eluted in 7.3 min. Recoveries from spiked stomach contents averaged 92%. The method can be used without modification for other alkaloids.

Liquid Chromatographic Determination of Sodium Fluoroacetate (Compound 1080) in Meat Baits and Formulations

1984 ◽  
Vol 67 (6) ◽  
pp. 1058-1061
Author(s):  
Harvey L Kramer
Keyword(s):  
Crown Ether ◽  
Chromatographic Determination ◽  
Reverse Phase ◽  
Ultraviolet Absorbance ◽  
Reverse Phase Column ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Phase Column

Abstract A liquid chromatographic (LC) method is described for the determination of sodium fluoroacetate in meat baits and formulations. Baits were extracted with water, ultrafiltered, partitioned into butanone, back-partitioned into dilute base, and diluted with acetonitrile. Aqueous formulations of 1080 were diluted with acetonitrile. The solutions were esterified with p-bromophenacyl bromide, using crown ether catalysis, and chromatographed on a 10 μm reverse phase column. Ultraviolet absorbance was monitored at 260 nm. Samples spiked to contain 1 mg and 10 mg 1080/100 g meat gave recoveries of 84.0-103.4%.

Liquid Chromatographic Determination of Clobetasone-17-Butyrate in Ointments

1990 ◽  
Vol 73 (6) ◽  
pp. 893-895 ◽  
Author(s):  
Ajay G Patel ◽  
Ramanbhai B Patel ◽  
Mukeshbhai R Patel
Keyword(s):  
Sodium Salt ◽  
Mobile Phase ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Reverse Phase ◽  
Reverse Phase Column ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Phase Column

Abstract A liquid chromatographic (LC) method has been developed for determination of clobetasone-17-butyrate In ointment using clobetasone propionate as an internal standard. Separation was carried out on a C18 reverse-phase column using water-methanol as a mobile phase. Methylparaben and propylparaben (both sodium salt) used as preservatives did not Interfere with separation. Compounds are detected photometrically at 235 nm. Mean assay results for 0.05% commercial ointments were 100.36% (n = 5). Mean recovery of clobetasone-17-butyrate added to commercial ointment was 99.89%.

Liquid Chromatographic Determination of Zoalene in Medicated Feeds

1984 ◽  
Vol 67 (5) ◽  
pp. 861-862 ◽  
Author(s):  
John Morawski ◽  
Glenn Kyle
Keyword(s):  
Colorimetric Method ◽  
Chromatographic Determination ◽  
Activated Alumina ◽  
Reverse Phase ◽  
Liquid Chromatographic Determination ◽  
Phase Liquid ◽  
Aoac Official ◽  
Liquid Chromatographic ◽  
Medicated Feeds

Abstract A rapid, reliable separation and quantitation of zoalene (3,5-dinitroo-toluamide) from feeds is accomplished by using reverse phase liquid chromatography (LC) and ultraviolet detection. An extraction technique which is similar to the present AOAC official colorimetric method is used before chromatographic analysis. This extraction is followed by an activated alumina cleanup and LC to separate zoalene from feed matrix. The methodology was applied to a variety of spiked feed matrices, and yielded good recoveries. Liquid chromatographic results were shown to correlate with colorimetric determinations.

Reverse Phase Liquid Chromatographic Determination of Chlorophacinone and Diphacinone in Bait Formulations

1982 ◽  
Vol 65 (4) ◽  
pp. 927-929
Author(s):  
Brian R Bennett ◽  
Gregory S Grimes
Keyword(s):  
Acetic Acid ◽  
Glacial Acetic Acid ◽  
Chromatographic Determination ◽  
Reverse Phase ◽  
Target Concentration ◽  
External Standard ◽  
Liquid Chromatographic Determination ◽  
Phase Liquid ◽  
Liquid Chromatographic

Abstract Chlorophacinone and diphacinone are extracted at the 0.005% level from grain or paraffinized baits with glacial acetic acid. The target concentration is 0.01 mg/mL. The filtered supernate is chromatographed on a Partisil PXS ODS10/25 liquid chromatography column with premixed and degassed glacial acetic acid-tetrahydrofuran-water (14 + 2 + 9) and detected at 288 nm. The concentration is calculated by using an external standard. The recovery from spiked samples averaged 96.6% for both analytes. The response is linear from 0.001 to 0.040 mg/mL. The coefficient of variation of within-day replicates ranged from 1.1 to 2.5%.

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 Sulfite in Grapes and Selected Grape Products

1989 ◽  
Vol 72 (6) ◽  
pp. 903-906
Author(s):  
Gracia A Perfetti ◽  
Frank L Joe ◽  
Gregory W Diachenko
Keyword(s):  
Chromatographic Determination ◽  
Reverse Phase ◽  
Nitrobenzoic Acid ◽  
Tetrabutylammonium Ion ◽  
Aqueous Formaldehyde Solution ◽  
Liquid Chromatographic Determination ◽  
Aoac Official ◽  
Liquid Chromatographic ◽  
Aqueous Formaldehyde

Abstract A liquid chromatographic (LC) method is described for the determination of sulfite in grapes and certain grape products. Sulfite is extracted from grapes with aqueous formaldehyde solution buffered at pH 5; free sulfite is converted to hydroxymethylsulfonate (HMS), which is extremely stable at pH 3-7. Subsequent heating to 80°C for 30 min converts reversibly bound forms of sulfite to HMS. The extract is then analyzed by reverse-phase ion-pairing liquid chromatography, using a Cjg column and a mobile phase of aqueous 0.005M tetrabutylammonium ion in 0.05M acetate, pH 4.7, and a flow rate of 1 mL/min. Aqueous KOH is added to the eluate to convert HMS to free sulfite, which is then treated with 5,5'-dithiobis[2-nitrobenzoic acid]. This reaction produces the 3-carboxy-4-nitrothiophenolate anion, which is determined by measurement of electronic absorption at 450 nm. For grapes spiked with HMS at 5-20 ppm (as S02), recoveries ranged from 92 to 112%, with a coefficient of variation of 4.6%. The method was also used to determine sulfite in various grape products. Results were comparable to those obtained by the AOAC official Monier-Williams method.

Liquid Chromatographic Determination of Cinnamic and Benzoic Acids in Benzoin Preparations

1987 ◽  
Vol 70 (4) ◽  
pp. 689-691
Author(s):  
Abdel-Aziz M Wahbi ◽  
Mohammad A Abounassif ◽  
El-Rasheed A Gad-Kariem ◽  
Mahmoud W Ibrahim
Keyword(s):  
Chromatographic Determination ◽  
Cinnamic Acids ◽  
Reverse Phase ◽  
British Pharmacopoeia ◽  
Liquid Chromatographic Method ◽  
Individual Determination ◽  
Liquid Chromatographic Determination ◽  
The Individual ◽  
Liquid Chromatographic

Abstract A liquid chromatographic method for the individual determination of benzoic and cinnamic acids in 2 benzoin preparations is presented. The method specifies a reverse phase column and 0.01M KH2P04- methanol (85 + 15) as mobile phase at a flow rate of 1.8 mL/min, with detection at 254 nm. The method has been applied to 2 benzoin preparations and the results were compared with those from the British Pharmacopoeia method.

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.

Liquid Chromatographic Determination of Acetaminophen in Multicomponent Analgesic Tablets

1984 ◽  
Vol 67 (2) ◽  
pp. 339-341
Author(s):  
David J Krieger
Keyword(s):  
Chromatographic Determination ◽  
Ultraviolet Region ◽  
Active Components ◽  
Chlorpheniramine Maleate ◽  
Reverse Phase ◽  
Phenylephrine Hydrochloride ◽  
Photometric Detection ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A simple, rapid LC method is presented for the separation and determination of acetaminophen in analgesic preparations containing up to 6 additional active components. The method uses a C18 reverse phase column, methanol–0.75% acetic acid (1 + 3) mobile phase, and photometric detection in the ultraviolet region. Acetaminophen was effectively separated from chlorpheniramine maleate, phenylephrine hydrochloride, caffeine, salicylamide, aspirin, and phenacetin, as well as from salicylic acid, a degradation product of aspirin. Typical chromatograms of the separation of acetaminophen from the above compounds in synthetic mixture and in commercial multicomponent analgesic preparations are presented, along with reproducibility and recovery data.

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