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A facile and economical method for the quantitative analysis of melamine in rat plasma and its application to pharmacokinetic study

【摘要】:正In the last two years,melamine(MEL) attracted a wide-spread attention because of the acute renal failure caused by contamination of it in infant formula.The aim of this study is to establish a simple,rapid and economical method for the quantitative determination of MEL in rat plasma for further pharmacokinetic study.A triple quadrupole LC-MS/MS method is presented for the analysis.The method employed a simple protein sample treatment by precipitation with acetonitrile,centrifugation and dilution.The chromatographic separation was achieved on a zwitterionic ZIC(?)-HILIC column using isocratic elution at a flow rate of 0.1 mL/min over a total run time of 8 min.The column temperature was 35℃.The mobile phase consisted of an aqueous buffer(containing 5mM ammonium acetate and 0.2%acetic acid) and methanol(20:80,V/V).Mass spectrometric data were acquired in positive ion mode with the following parameters:spray voltage:3800 V;sheath gas pressure:30 Arbitrary units(Arb.);auxiliary gas pressure:10 Arb.;capillary temperature:350℃.Quantification was performed with selected reaction monitoring(SRM) with(m/z)~+ 127.0→85.1(collision energy 19 eV) for MEL. The method was linear over the range of 10-1000 ng/mL(R = 0.999).The intra- and inter-day precisions ranged from 1.6%to 5.8%and 1.3 to 4.7%, respectively.Meanwhile,the intra- and inter-day accuracies were 99.1%- 109%) and 95.0-105%,respectively.All the other validation data were within the required limits.The method was successfully applied to the evaluation of pharmacokinetic properties of MEL in rats,which is supposed to be meaningful to reveal the toxicity mechanism.

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