Improved Method for High Pressure Liquid Chromatographic Determination of Chlorophacinone in Mouse Tissue

1982 ◽  
Vol 65 (6) ◽  
pp. 1299-1301
Author(s):  
Joseph B Addison
Keyword(s):  
High Pressure ◽  
Chromatographic Determination ◽  
Peak Height ◽  
Mouse Tissue ◽  
Height Measurement ◽  
Liquid Chromatograph ◽  
Order Of Magnitude ◽  
High Pressure Liquid Chromatograph ◽  
Liquid Chromatographic

Abstract A simplified method is described for the determination of chlorophacinone, 2-[(p-chlorophenyl)- phenylacetyl]-l,3-indandione, in homogenized mice. Chlorophacinone is extracted with acetonitrile. After Florisil cleanup, the extract is injected into a high pressure liquid chromatograph for reverse phase chromatography on a polar Lichrosorb NH2 (10 μm) column, with a mobile phase of acetonitrile-water (80 + 20). An injection containing 70 ng chlorophacinone produces 1/2 scale peaks at 254 nm with a full scale absorbance of 0.1 unit, an order of magnitude improvement over the sensitivity reported earlier with a 280 nm detector. Six homogenized mice samples and six spiked homogenized mice samples were quantitatively analyzed for trace levels of chlorophacinone by this method. Recoveries from spiked samples, as determined by peak height measurement, were >95%. Mean retention time for the chlorophacinone peaks in all samples was 6.05 ± 0.05 min. Chlorophacinone levels determined in homogenized whole mouse samples ranged from 0 to 63 ppm.

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 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 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 Theobromine and Caffeine in Cocoa and Chocolate Products: Collaborative Study

1980 ◽  
Vol 63 (3) ◽  
pp. 591-594
Author(s):  
Wesley R kreiser ◽  
Robert A Martin ◽  
◽  
R Bigornia ◽  
R Bond ◽  
...  
Keyword(s):  
High Pressure ◽  
Petroleum Ether ◽  
Collaborative Study ◽  
Chromatographic Determination ◽  
Peak Height ◽  
High Pressure Liquid Chromatographic ◽  
Liquid Chromatographic Determination ◽  
The Mean ◽  
Liquid Chromatographic

Abstract Four duplicate samples of cocoa-containing materials, a practice sample, and standards were submitted to the collaborators for theobromine and caffeine analysis by HPLC. In the method the samples are defatted with petroleum ether, and dried. The fat-free residue is then extracted with water and an aliquot is injected into the chromatograph. Compounds are quantitated by comparison with internal or external standards, either by peak height or peak area. Results for all the analyses showed that few of the values were more than 2 standard deviations from the mean. The method has been adopted as official first action.

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.

High Pressure Liquid Chromatographic Determination of 3,5-Dimethyl-4-(Methylthio) phenyl Methylcarbamate in Formulations

1979 ◽  
Vol 62 (1) ◽  
pp. 5-7
Author(s):  
Martha Fuzesi
Keyword(s):  
High Pressure ◽  
Quantitative Measurement ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Peak Height ◽  
Pesticide Formulations ◽  
Liquid Chromatographic Determination ◽  
Commercial Pesticide ◽  
Liquid Chromatographic

Abstract Methiocarb (3,5 - dimethyl - 4 - (methylthio) - phenyl methylcarbamate) is extracted from commercial pesticide formulations with methanol, and carbaryl is added as an internal standard. The sample is chromatographed by reverse phase high pressure liquid chromatography, with ultraviolet detection at 254 nm. Peak height ratios are used for quantitative measurement. The method is rapid and accurate, and recoveries from laboratory-prepared formulations averaged 100.8%.

High Pressure Liquid Chromatographic Determination of Mannitol and Sorbitol in Sugarless Chewing Gums

1977 ◽  
Vol 60 (6) ◽  
pp. 1318-1320
Author(s):  
Eugene C Samarco
Keyword(s):  
High Pressure ◽  
Membrane Filter ◽  
Cation Exchange Resin ◽  
Chromatographic Determination ◽  
Phase System ◽  
High Pressure Liquid Chromatographic ◽  
Liquid Chromatograph ◽  
Chewing Gums ◽  
Liquid Chromatographic

Abstract A precise and accurate high pressure liquid chromatographic method is presented for the simultaneous separation and determination of mannitol and sorbitol in sugarless chewing gums. The 2 isomers are extracted into water, using a 2-phase system to facilitate dissolution of the chewing gum. The aqueous phase is filtered through a 0.45 μm pore membrane filter and injected into the liquid chromatograph. The mannitol and sorbitol are eluted from an Aminex Q-15S cation exchange resin with water as the mobile phase and are quantitated by using a differential refractive index detector. Average recoveries for mannitol and sorbitol are 98.9 and 99.2%, respectively.

Reverse Phase High Pressure Liquid Chromatographic Determination of Arprinocid in Animal Feeds

1982 ◽  
Vol 65 (1) ◽  
pp. 43-47
Author(s):  
Virginia A Thorpe
Keyword(s):  
High Pressure ◽  
Chromatographic Determination ◽  
Peak Height ◽  
Reverse Phase ◽  
High Pressure Liquid Chromatographic ◽  
Simple Method ◽  
Working Standard ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A simple method is presented for determination of arprinocid in finished feeds by reverse phase high pressure liquid chromatography. The sample is extracted with 95% DMF, the major feed interferences are removed by alumina chromatography, and arprinocid is separated from the remaining interferences on the HPLC column. The peak height detected at 254 nm can be quantitated by direct comparison with the working standard.

High Pressure Liquid Chromatographic Determination of Satratoxins G and H in Cereal Grains

1980 ◽  
Vol 63 (6) ◽  
pp. 1278-1281 ◽  
Author(s):  
Michael E Stack ◽  
Robert M Eppley
Keyword(s):  
High Pressure ◽  
Silica Gel ◽  
Limit Of Detection ◽  
Chromatographic Determination ◽  
Chloroform Extract ◽  
Cereal Grains ◽  
High Pressure Liquid Chromatographic ◽  
Liquid Chromatograph ◽  
Liquid Chromatographic

Abstract A high pressure liquid chromatographic (HPLC) method is described for the detection and quantitative determination of satratoxins G and H in cereal grains. The toxins are extracted from the sample by blending with methanol-water (55+45) in the presence of hexane, followed by partitioning into chloroform. The chloroform extract is further purified on a 10 g silica gel column. A high pressure liquid chromatograph, equipped with a microparticle silica gel column and a 254 nm absorbance detector, is used for the determination. Additional confirmation of identity is obtained by mass spectrometry or by a brine shrimp bioassay of the HPLC eluates corresponding to the retention times of satratoxins G and H. The recoveries of added satratoxins G and H from wheat samples averaged 65% for G and 71% for H (200–1000 mg/kg). The coefficients of variation (CV) were 15% for G and 14% for H. The lower limit of detection was 200 μg/kg for wheat. Analysis of corn, oats, and barley samples (400 μg/kg of each toxin added) gave comparable recoveries. Only the corn extract exhibited HPLC interferences at the retention time for satratoxin H. The method was also used to analyze samples of corn, oats, wheat, barley, and rice on which Stachybotrys atra had been cultured.

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.

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