Liquid Chromatographic Determination of Aflatoxicol in Porcine Liver

1987 ◽  
Vol 70 (3) ◽  
pp. 475-478
Author(s):  
Krystyna Tyczkowska ◽  
James E Hutchins ◽  
Winston M Hagler
Keyword(s):  
Limit Of Detection ◽  
Chromatographic Determination ◽  
Porcine Liver ◽  
Liver Sample ◽  
Aqueous Fraction ◽  
Silica Cartridge ◽  
Liquid Chromatographic Determination ◽  
Phase Liquid ◽  
Liquid Chromatographic

Abstract A liquid chromatographic (LC) method for determination of aflatoxicol in porcine liver was developed. Liver sample is homogenized with water, diluted with saturated Na2S04 solution, and extracted with acetone. After filtration, less polar interferences are removed by partition with isooctane. Aflatoxicol in the aqueous fraction is partitioned into CHC13. The extract is dried over anhydrous Na2S04 and evaporated nearly to dryness at 35°C under a gentle flow of dry filtered air or nitrogen. Residue is dissolved in CHCl3-hexane and applied to a hexane-activated silica cartridge. The cartridge is washed with hexane-CHClj, then aflatoxicol is eluted with CHCl3-acetone. Purified extract is evaporated to dryness, dissolved in methanol, and analyzed by C18 reverse phase liquid chromatography using a water- CHjCN-acetic acid mobile phase and fluorescence detection. Recovery of aflatoxicol from spiked liver samples at levels ranging from 0.25 to 4.0 ng aflatoxicol/g wet tissue averaged 92% with a limit of detection of about 0.1 ng aflatoxicol/g liver.

Matrix Solid-Phase Dispersion Extraction and Liquid Chromatographic Determination of Ivermectin in Bovine Liver Tissue

1992 ◽  
Vol 75 (4) ◽  
pp. 655-658 ◽  
Author(s):  
Frank J Schenck ◽  
Steven A Barker ◽  
Austin R Long
Keyword(s):  
Methylene Chloride ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Bovine Liver ◽  
Chromatographic Determination ◽  
Liver Sample ◽  
Antiparasitic Drug ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A method for the isolation and liquid chromatographic (LC) determination of the antiparasitic drug ivermectin in bovine liver is presented. Liver samples (0.5 g) are blended with 2 g C18 (octadecylsilylderivatized silica packing material). A column made from the C18liver matrix is washed with 3 mL hexane, then the ivermectin is eluted with methylene chloride-ethyl acetate (3 + 1). After purification by alumina solid-phase extraction, the ivermectin is derivatized and analyzed by LC with fluorescence detection. The overall recovery of ivermectin added to liver was 74.6%. The lowest level validated in tissue by the method was 10 ppb, and the limit of detection was 1 ppb. This method and a classical extraction method gave comparable results for a liver sample that contained incurred ivermectin residues. The method uses small volumes of solvents, has a limited number of sample manipulations, and does not require solvent partitioning or backwashing of extracts. These characteristics make this method attractive when compared to classical isolation procedures for ivermectin.

Rapid Liquid Chromatographic Determination of Aflatoxins in Heavily Contaminated Corn

1983 ◽  
Vol 66 (6) ◽  
pp. 1458-1465 ◽  
Author(s):  
James E Hutchins ◽  
Winston M Hagler
Keyword(s):  
Chromatographic Determination ◽  
Mean Value ◽  
Reverse Phase ◽  
Silica Cartridge ◽  
Aoac Method ◽  
Precision Study ◽  
Liquid Chromatographic Determination ◽  
Phase Liquid ◽  
Liquid Chromatographic

Abstract A procedure is described for rapid, quantitative determination of aflatoxins B1, B2, G1, and G2 in heavily contaminated corn (>500 μg B1/kg) from field, greenhouse, and growth chamber experiments employing artificial inoculation of corn with Aspergillus flavus. Whole kernel corn is ground to pass a 1 mm screen and mixed before extraction of a water-wetted (25 mL) 50 g subsample with 250 mL chloroform. The filtered extract is diluted 1:1 with hexane and applied to a hexane-wetted (10 mL) disposable silica cartridge. Interferences are removed with chloroform-hexane (1 + 3), and aflatoxins are quantitatively eluted with hexane-acetone (1 + 1). Aflatoxins B1 and G1 are converted to the more intensely fluorescent hemiacetals, B2a and G2a, by treatment with trifluoroacetic acid-water. Derivatized aflatoxins are separated by reverse phase liquid chromatography (LC) and quantitated fluorometrically. Compared with AOAC method I (CB) for corn, using samples containing approximately 50 and 10 000 μg B1/kg, agreement between methods was good at the lower level while the rapid method yielded a considerably larger mean at the higher level. A precision study of 30 replicate samples produced a coefficient of variation of 8.46% at a mean value of 1066 μg B1/kg. The cartridge method was developed for LC analysis of samples that contain >500 μg aflatoxin B1/kg corn, but it may be used to quantitate as little as 10 μg B1/kg with no modification.

Reverse-Phase Liquid Chromatographic Determination of Benzoic and Sorbic Acids in Fresh Cheese

1988 ◽  
Vol 71 (5) ◽  
pp. 1068-1071 ◽  
Author(s):  
Frans J. E. M Kuppers ◽  
Jan A Jans
Keyword(s):  
Limit Of Detection ◽  
Chromatographic Determination ◽  
Acetate Buffer ◽  
Reverse Phase ◽  
Effluent Flow Rate ◽  
Fresh Cheese ◽  
Liquid Chromatographic Determination ◽  
Phase Liquid ◽  
Liquid Chromatographic

Abstract The sorbate and benzoate contents of commercial fresh cheese (quarg) samples are determined by reverse-phase liquid chromatography following extraction with a methanol-acetate buffer pH 4.5 mixture (37 + 63). The mobile phase is acetonitrile-acetate buffer pH 4.5 (20 + 80), the effluent flow rate is maintained at 1.0 mL/min, and the detector is set at 232 nm. Recoveries from quarg spiked at the 5-50 mg/kg level ranged from 95 to 99%, which compares favorably with methods previously published. Precision averaged 2-5% RSD, whereas the limit of detection was 0.3 mg/kg (sorbic acid) and 1.0 mg/kg (benzoic acid).

Simultaneous Liquid Chromatographic Determination of Fenamiphos and Its Metabolites in Soil

1992 ◽  
Vol 75 (1) ◽  
pp. 62-65 ◽  
Author(s):  
R Khazanchi ◽  
S Walia ◽  
S K Handa
Keyword(s):  
Chromatographic Method ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Chromatographic Determination ◽  
Reversed Phase ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic Determination ◽  
Phase Liquid ◽  
Liquid Chromatographic

Abstract A reversed-phase liquid chromatographic method has been developed for the determination of fenamiphos and the metabolites fenamiphos sulfoxide, fenamiphos sulfone, 3-methyl-4-(methylthlo)- phenol, and 3-methyl-4-(methylsulflnyl)phenol. Trace quantities of the nematlclde and Its metabolites In soil can be determined simultaneously. The limit of detection of the method was 5 ppm. Recoveries of fenamiphos and Its degradation products at fortification levels of 25,50, and 100 ppm ranged from 99.2 to 100.8%. Standard deviations ranged from 0.29 to 0.70 ppm.

Liquid Chromatographic Determination of Aflatoxins in Feedstuffs Containing Citrus Pulp

1988 ◽  
Vol 71 (5) ◽  
pp. 957-961 ◽  
Author(s):  
Walter E Paulsch ◽  
Eric A Sizoo ◽  
Hans P Van Egmond
Keyword(s):  
Limit Of Detection ◽  
Chromatographic Determination ◽  
Reverse Phase ◽  
Citrus Pulp ◽  
Coefficients Of Variation ◽  
Liquid Chromatographic Determination ◽  
Phase Liquid ◽  
Liquid Chromatographic ◽  
Postcolumn Derivatization

Abstract A liquid chromatographic (LC) method was developed for the determination of aflatoxins in feedstuffs containing citrus pulp. The feedstuff sample is extracted with chloroform, followed by Sep-Pak Florisil cartridge cleanup and Sep-Pak C18 cartridge cleanup. The final eluate (water-acetone, 85 + 15, v/v) is submitted to reverse-phase liquid chromatography with water-methanol-acetonitrile (130 + 70 + 40, v/v/v) as mobile phase and postcolumn derivatization with iodine. Citrus components are removed from the extract efficiently. The limit of detection for aflatoxin B1 is< 1 μg/kg. Other aflatoxins can also be detected and measured. Recoveries of aflatoxins B1 B2, G,1 and G2 for dairy rations spiked at 13, 5, 10, and 4 μg/kg were 87, 86, 81, and 82%, respectively. Corresponding coefficients of variation were 3.1, 3.6, 5.2, and 3.8%, respectively.

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%.

scholarly journals Liquid Chromatographic Determination of α-Solasonine in Frozen Green Peas as an Indicator of the Presence of Nightshade Berries

2003 ◽  
Vol 86 (4) ◽  
pp. 759-763 ◽  
Author(s):  
Peter Cavlovic ◽  
Mohan Mankotia ◽  
Peter Pantazopoulos ◽  
Peter M Scott
Keyword(s):  
Limit Of Detection ◽  
Chromatographic Determination ◽  
Solanum Nigrum ◽  
Expanded Uncertainty ◽  
Method Performance ◽  
Limit Of Quantitation ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Green Peas

Abstract Nightshade berries containing glycoalkaloids can be a contaminant in green peas. Methodology was developed to detect this contamination. The glycoalkaloid α-solasonine was extracted from frozen green peas with 1% (v/v) acetic acid, cleaned up on a C18 cartridge, and determined by liquid chromatography with UV detection at 200 nm. Method performance characteristics for the determination of α-solasonine include linearity from 140 to 1500 ng injected (r = 0.9996–0.9999); recovery ranging from 68 to 79%; limit of quantitation (LOQ) = 4.5 ppm (280 ng standard), and limit of detection = 0.64 ppm (40 ng standard). At the LOQ, the expanded uncertainty at 95% confidence was 0.38 × the reported value. The method was applied to the detection of α-solasonine in frozen green peas in a 2-year study of 60 samples of frozen green peas from Ontario, Canada. None of the samples contained α-solasonine. No unripe berries of Solanum nigrum were detected visually in the samples.

Liquid Chromatographic Determination of Carminic Acid in Yogurt

1989 ◽  
Vol 72 (2) ◽  
pp. 231-234 ◽  
Author(s):  
Mercedes Jalón ◽  
Majesús Peńa ◽  
Julián C Rivas
Keyword(s):  
Chromatographic Determination ◽  
Carminic Acid ◽  
Reverse Phase ◽  
Liquid Chromatographic Method ◽  
Relative Standard ◽  
Array Detection ◽  
Liquid Chromatographic Determination ◽  
Phase Liquid ◽  
Liquid Chromatographic

Abstract A reverse-phase liquid chromatographic method is described for the determination of carminic acid in yogurt. A C18 column is used with acetonitrile-1.19M formic acid (19 + 81) as mobile phase and diode array detection. Sample preparation includes deproteinization with papain and purification in a polyamide column. The relative standard deviation for repeated determinations of carminic acid in a commercial strawberry-flavored yogurt was 3.0%. Recoveries of carminic acid added to a natural-flavored yogurt ranged from 87.2 to 95.3% with a mean of 90.2%. The method permits measurement of amounts as low as 0.10 mg/kg.

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