High Pressure Liquid Chromatographic Determination of Chlorophacinone in Formulations

1979 ◽  
Vol 62 (5) ◽  
pp. 1001-1003
Author(s):  
Ralph G Grant ◽  
Richard K Pike
Keyword(s):  
High Pressure ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Whole Grain ◽  
High Pressure Liquid Chromatographic ◽  
Liquid Chromatograph ◽  
High Pressure Liquid Chromatograph ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A simple and rapid method is described determining for 2- ((p-chlorophenyl) phenylacetyl-1,3- indandione (chlorophacinone) in rodenticides formulated as tracking powders and whole grain and crushed grain baits. The bait is extracted with methanol containing an internal standard, and the extract is injected into a high pressure liquid chromatograph. The sample is analyzed by reverse phase chromatography on octadecyl (C18) bonded to glass beads with a mobile phase of methanolwater (35+65) plus 0.75% NH4OH. A 5 μL injection containing 240 ng benzophenone internal standard and 77 ng chlorophacinone produces half scale peaks at 280 nm with a full scale absorbance of 0.01 absorbance unit. Two formulations and a spiked sample were analyzed by the method. Recovery as determined by peak area was >97%.

High Pressure Liquid Chromatographic Determination of Xanthomegnin in Corn

1978 ◽  
Vol 61 (3) ◽  
pp. 590-592
Author(s):  
Michael E Stack ◽  
Nathan L Brown ◽  
Robert M Eppley
Keyword(s):  
High Pressure ◽  
Silica Gel ◽  
Chromatographic Determination ◽  
High Pressure Liquid Chromatographic ◽  
Liquid Chromatograph ◽  
High Pressure Liquid Chromatograph ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Layer Chromatography

Abstract A method is described for the detection and quantitative analysis of xanthomegnin in corn samples. Initial extraction with CHCI3 in the presence of 0.5M H3PO4 is followed by additional purification using silica gel column chromatography. A high pressure liquid chromatograph equipped with a microparticle silica gel column and a 405 nm absorbance detector is used for detection and quantitation of the xanthomegnin. The identity of xanthomegnin is confirmed by thin layer chromatography on silica gel plates developed with benzenemethanol- acetic acid (90-(-5+5). The recovery of xanthomegnin added to corn samples at levels of 0.75–9.6 mg/kg averaged 41% with a coefficient of variation of 25%.

High Pressure Liquid Chromatographic Determination of N-3-Pyridylmethyl-N′-p-nitrophenylurea in Rodenticides

1977 ◽  
Vol 60 (6) ◽  
pp. 1375-1378
Author(s):  
Carl W Sims ◽  
Richard K Gard
Keyword(s):  
High Pressure ◽  
Methylene Chloride ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Liquid Chromatograph ◽  
Two Samples ◽  
High Pressure Liquid Chromatograph ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A simple and rapid method is described for determining N′-3-pyridylmethyl-N′-p-nitrophenylurea (RH-787) in Vacor Ratkiller rodenticide. The bait is extracted with acetone, the extract is evaporated to dryness, an internal standard is added, and the solution is injected into a high pressure liquid chromatograph. The sample is analyzed by normal phase chromatography on a Partisil 10 column with a mobile phase of methanol-methylene chloride (10+90). An 8 μl injection containing 4 μg pyridine internal standard and 8 μg RH-787 produces half-scale peaks at 254 nm with a full scale absorbance of 0.5 absorbance unit. In an alternative procedure, the active ingredient is extracted from the bait with acetone and titrated to a methyl red end point with 0.1N perchloric acid dissolved in acetic acid. Two samples of Vacor Ratkiller and a spiked blank were analyzed by both procedures.

High Pressure Liquid Chromatographic Determination of Physostigmine Salicylate and Physostigmine Sulfate in Liquids and Ointments: Collaborative Study

1982 ◽  
Vol 65 (1) ◽  
pp. 132-137
Author(s):  
Norlin W Tymes ◽  
◽  
G Briguglio ◽  
C Corcoran ◽  
R Everett ◽  
...  
Keyword(s):  
High Pressure ◽  
Collaborative Study ◽  
Internal Standard ◽  
Pharmaceutical Formulations ◽  
Chromatographic Determination ◽  
Reverse Phase ◽  
High Pressure Liquid Chromatographic ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract Results of 11 laboratories are presented for the collaborative study of a proposed method for the quantitative reverse phase high pressure liquid chromatographic (HPLC) determination of physostigmine salicylate and physostigmine sulfate in pharmaceutical formulations. The samples consisted of commercial solution, injection, and ointment preparations, each containing one of the physostigmine salts. The physostigmine salt is extracted from ointments with acetonitrile after the ointment is dissolved in hexane. Liquid preparations are diluted directly. Physostigmine is determined at 254 nm on a C18 column by comparison with a physostigmine standard. Flurazepam hydrochloride is the internal standard. The method has been adopted official first action for the solution dosage form.

High Pressure Liquid Chromatographic Determination of Nitrofurazone in Milk

1979 ◽  
Vol 62 (1) ◽  
pp. 19-22 ◽  
Author(s):  
Arnost B Vilim ◽  
Agnes I Macintosh
Keyword(s):  
High Pressure ◽  
Screening Method ◽  
Chromatographic Determination ◽  
Organic Layer ◽  
High Pressure Liquid Chromatographic ◽  
Liquid Chromatograph ◽  
Milk Serum ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A rapid high pressure liquid chromatographic (HPLC) screening method for the quantitative determination of nitrofurazone in milk has been developed. The drug is extracted with ethyl acetate from a 2.0 ml milk serum sample, the organic layer is evaporated to dryness, and the residue is dissolved in the mobile phase and injected into the liquid chromatograph. A reverse phase μBondapak C18 column is used with monitoring at 365 nm. The detection limit is 5 ppb and recoveries are 57—67%. Mass spectroscopic confirmation of the HPLC nitrofuran peak is described.

Simultaneous high-pressure liquid-chromatographic determination of some anticonvulsants in serum.

1976 ◽  
Vol 22 (1) ◽  
pp. 25-31 ◽  
Author(s):  
R F Adams ◽  
F L Vandemark
Keyword(s):  
High Pressure ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Serum Samples ◽  
Reverse Phase ◽  
High Pressure Liquid Chromatographic ◽  
Peak Areas ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract We describe procedures for simultaneously determining some anticonvulsants (phenobarbital, diphenylhydantoin, primidone, ethosuximide, methsuximide, carbamazepine) in serum by high-pressure liquid chromatography. The drugs, together with an internal standard, phenacetin, are adsorbed from serum onto charcoal and eluted from it with organic solvent. The eluate is analyzed isocratically on a reverse-phase column with a mobile phase consisting of acetonitrile/water (17/83 by volume). The eluted drugs are detected by their absorption at 195 nm, and quantities estimated from their peak areas as compared with those of extracted standards. Results are reproducible to about 6%. Sensitivities, for 0.5-ml serum samples, of 0.1 mg/liter for all the drugs analyzed except ethosuximide (0.5 mg/liter) are attained routinely. Correlation of results with gas chromatography was 0.912 for phenobarbital, 0.982 for diphenylhydantoin, 0.886 for primidone, and 0.966 for ethosuximide. Amobarbital and secobarbital interfere with the analysis; chlordiazepoxide, methaqualone, salicylate, diazepam, and oxazepam do not. Including extraction, analysis time for a single sample is 20 min.

High Pressure Liquid Chromatographic Determination of Difenzoquat in Formulations

1980 ◽  
Vol 63 (3) ◽  
pp. 647-649
Author(s):  
Carla Barry ◽  
Richard K Pike
Keyword(s):  
High Pressure ◽  
Quantitative Measurement ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
High Pressure Liquid Chromatographic ◽  
Pesticide Formulations ◽  
Liquid Chromatographic Determination ◽  
Commercial Pesticide ◽  
Liquid Chromatographic

Abstract Difenzoquat (l,2-dimethyl-3,5-diphenylpyrazolium ion) as its methyl sulfate is extracted from commercial pesticide formulations with acetonitrile-water (1+), with acetophenone added as internal standard. The sample is chromatographed by reverse phase high pressure liquid chromatography with ultraviolet detection at 280 nm. Peak area ratios are used for quantitative measurement. The method is simple, rapid, and direct, and its applicability to other quaternary ammonium herbicides is discussed.

High Pressure Liquid Chromatographic Determination of Phenol in Honey

1981 ◽  
Vol 64 (2) ◽  
pp. 337-339
Author(s):  
Peter Sporns
Keyword(s):  
High Pressure ◽  
Mobile Phase ◽  
Silicic Acid Column ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Peak Height ◽  
High Pressure Liquid Chromatographic ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A method is described for determining phenol in honey by using high pressure liquid chromatography (HPLC). An internal standard, 2-phenylethanol, was added to honey which was steam-distilled and chromatographed on a 25 cm × 3.2 mm id Spherisorb 5 µm silicic acid column using water as the mobile phase. Absorbance was monitored at 195 nm. Using a mixed standard of known concentration and peak height measurements, the amount of phenol in the honey could be quantitated. Recovery of added phenol was checked at levels from 0.1 to 33 ppm.

High Pressure Liquid Chromatographic Determination of Capsaicin in Oleoresin and Personal Protection Aerosols

1983 ◽  
Vol 66 (5) ◽  
pp. 1304-1306
Author(s):  
Mark W Law
Keyword(s):  
High Pressure ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Personal Protection ◽  
High Pressure Liquid Chromatographic ◽  
Liquid Chromatographic Method ◽  
Hot Peppers ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A simple and accurate high pressure liquid chromatographic method has been developed for determination of capsaicin in oleoresin capsicum and mineral oil-based aerosol formulations intended for personal protection. Capsaicin, the main ingredient responsible for the spicy pungency of various hot peppers and paprika, is extracted with acetonitrile and aliquots are analyzed on a 10 μm C18 column at 280 nm with acetonitrile-water (45 + 55) mobile phase. Dihydrocapsaicin is also extracted and is simultaneously quantitated with propiophenone as an internal standard.

High Pressure Liquid Chromatographic Determination of Supplemental Methionine in Poultry Premix

1982 ◽  
Vol 65 (1) ◽  
pp. 62-65
Author(s):  
Dubravka Matešič
Keyword(s):  
High Pressure ◽  
Mobile Phase ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Buffer Solution ◽  
Reverse Phase ◽  
High Pressure Liquid Chromatographic ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract Supplemental methionine was extracted from a feed sample with O.IM HCI and separated by reverse phase or ion-exchange high pressure liquid chromatography and isocratic elution with KH2PO4 buffer solution as the mobile phase. Methionine was detected at 205 nm. The most reliable results were obtained by using reverse phase chromatography, 0.05M KH2PO4 buffer at pH 2.6 as mobile phase, and tyrosine as internal standard.

High Pressure Liquid Chromatographic Determination of Sulfisoxazole in Pharmaceuticals and Separation Patterns of Other Sulfonamides

1981 ◽  
Vol 64 (4) ◽  
pp. 851-854
Author(s):  
Robert W Roos
Keyword(s):  
High Pressure ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
High Pressure Liquid Chromatographic ◽  
Liquid Chromatographic Method ◽  
Acetic Acid Water ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Good Agreement

Abstract A high pressure liquid chromatographic method has been developed for the identification and determination of sulf isoxazole in tablet, liquid, and ointment dosage forms. The method specifies a µBondapak C18 column, an acetonitrile-acetic acid-water (22.5 + 1 + 76.5) mobile phase, and ultraviolet detection at 254 nm. For quantitative purposes, sulfabenzamide is used as an internal standard. Commercial preparations were analyzed by the proposed method and results were compared with those obtained by the U.S. Pharmacopeia XIX and National Formulary XIV methods; good agreement was obtained. The elution behaviors of 19 additional sulfonamides were also established to verify the specificity of the proposed method for sulfisoxazole. These elutions patterns show potential for separation and identification of all 20 sulfonamides

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