A sensitive and reliable method using liquid chromatography-tandem mass spectrometry (LC-MS/MS) with an electrospray-positive ionization method was developed for the determination of aflatoxin M(1) in milk. This method includes simple extraction of the sample with acetonitrile by ultrasonic, separation on an MGIII-C(18) column using 0.01% formic acid buffer/acetonitrile (60 : 40, v/v) as mobile phase, and MS/MS detection using multiple reaction-monitoring mode. Average recoveries of aflatoxin M(1) from spiked samples at concentrations of 0.02 and 1 ng ml(-1) ranged from 77% to 94%, with a 6% relative standard deviation. The limit of detection and limit of quantification were 0.006 and 0.02 ng ml(-1), respectively. The standard curve was linear between 0.02 and 20.0 ng ml(-1). The recommended method is simple, rapid, specific and reliable for the routine monitoring of aflatoxin M(1) in milk.
A reliable, rapid, and sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for simultaneous determination of chloramphenicol and aflatoxin M(1) in milk has been developed. This method includes simple extraction of sample with acetonitrile, separation on a MGIII-C(18) column using 5 mM ammonium acetate aqueous solution/methanol (60:40, v/v) as mobile phase, and MS/MS detection using multiple reaction monitoring mode. The method was validated according to Commission Decision 2002/657/EC. The limits of detection (LODs) were 0.05 μg/kg for chloramphenicol and 0.005 μg/kg for aflatoxin M(1.) The limits of quantification (LOQs) were 0.2 μg/kg for chloramphenicol and 0.02 μg/kg for aflatoxin M(1). The recovery values ranged from 88.8% to 100.6%, with relative standard deviation lower than 15% in all cases, when samples were fortified at three different concentrations. The decision limits (CCα) and detection capability (CCβ) of the method were also reported. This method has been successfully applied for simultaneous analysis of chloramphenicol and aflatoxin M(1) residues in milk from local supermarkets in China.
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