HPLC-MS/MS快速测定动物肌肉中6种聚醚类抗生素

Fast determination of polyether antibiotics residues in animal muscle tissues by high performance liquid chromatography tandem mass spectrometry

建立动物肌肉组织中6种聚醚类抗生素(莫能菌素、马杜拉霉素、盐霉素、和拉沙洛菌素、甲基盐霉素、尼日利亚菌素)的高效液相色谱-电喷雾串联质谱快速测定法。样品经乙腈提取,并以乙腈饱和的正己烷净化,采用甲酸水溶液-甲醇体系为流动相,梯度洗脱,电喷雾离子源正离子多反应监测模式进行质谱分析。结果表明,在优化的条件下对样品进行分析检测,各抗生素的回收率为88.0%～108.7%,RSD为2.3%～6.1%(C=10μg/kg,n=5),6种待测物在1.0～150ng/mL范围内均呈线性,线性回归系数R2均大于0.99,检出限为0.05～0.2μg/kg。该方法操作简单,灵敏度高,适用于动物肌肉组织中6种聚醚类药物的批量检测分析。

A high performance liquid chromatography electrospray ionization tandem mass spectrometry（HPLC-ESI MS/MS） method for the determination of six polyether antibiotics（monensin,maduramicin,salinomycin,lasalocid, narasin and nigericin） in animal muscle tissues was established.Polyether antibiotics in animal muscle tissues were extracted with acetonitrile and then cleaned up with n-hexane being saturated by acetonitrile.The analytes were separated using formic acid aqueous solution-methanol system as mobile phase with a linear gradient elution program,and the quantification was carried out by positive electrospray ionization and multiple reaction monitoring（MRM） mode.Under the optimized conditions,the average recoveries for six polyether antibiotics ranged from 88.0%～108.7%,the limits of detection were in the range of 0.05～0.2 μg/kg with precisions（RSDs（%）,C=10 μg/kg,n=5） ranging from 2.3% to 6.1%,and all of the analysis compounds exhibited good linearity over a range of 1.0～150 ng/mL with the correlation coefficient over 0.99.Experiment results showed that the method was simple,rapid,sensitive and was applicable to simultaneous determination of multi-residues of six polyether antibiotics in animal muscle tissues.