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Automated liquid chromatographic determination of aflatoxin M1 in milk using on-line dialysis for sample preparation.

A procedure has been developed for the automated isolation of aflatoxin M1 from decreamed milk. The method uses on-line stopped flow dialysis and subsequent trace enrichment on a reverse-phase column. After a back-flush to the analytical liquid chromatography column, aflatoxin M1 is determined with fluorescence detection. Fully automated analysis is possible with reproducible dialysis recoveries above 50% (CV = 7.5%, n = 25 at the 50 ng/kg level) and determination levels of 20 ng/kg within 20 min.

Aflatoxin M1↗

Simultaneous liquid-chromatographic determination of some bronchodilators, anticonvulsants, chloramphenicol, and hypnotic agents, with Chromosorb P columns used for sample preparation.

We describe a simple liquid-chromatographic system for simultaneously measuring bronchodilators, anticonvulsants, hypnotics, and chloramphenicol. Use in therapeutic drug monitoring includes determination of theophylline, caffeine, chloramphenicol, ethosuximide, primidone, phenobarbital, phenacemide, phenytoin, mephenytoin, nirvanol, and carbamazepine and its bioactive metabolites within 13 min. In the "toxicology mode" theophylline, caffeine, barbital, butabarbital, pentobarbital, amobarbital, secobarbital, primidone, phenobarbital, methylprylon, glutethimide, methaqualone, phenytoin, mephenytoin, nirvanol, and carbamazepine and its bioactive metabolites are resolved within 17 min. A reversed-phase C8 column (5-microns particles) is used, with acetonitrile/water (20/80 by vol) as mobile phase. The drugs are extracted from 50 microL of serum with use of a Chromosorb P microcolumn and chloroform/isopropanol (6/1 by vol). The drugs are quantified by absorbance at 208 nm, with tolylphenobarbital as internal standard. Lower limits of detection varied from 0.05 to 0.1 mg/L, analytical recovery from 94% to 106%; CVs were less than 5.6% within run, less than 6.9% between runs.

Anticonvulsants↗

Sampling and preparation of sample for chemical examination.

Sampling and methods for reducing a laboratory sample to a test sample are discussed, with particular emphasis on sampling peanuts for aflatoxin analysis as a practical example. The only way to control the total error in the analysis of this heterogeneous product is to take and to analyze many and large samples.

Aflatoxins↗