水产品中7种大环内酯类抗生素残留量的HPLC-MS/MS测定法

Determination of 7 macrolide antibiotic residues in aquatic products by HPLC-MS/MS

建立了水产品中7种大环内酯类抗生素[竹桃霉素(OLD)、红霉素(ERM)、吉他霉素(KIT)、交沙霉素(JOS)、螺旋霉素(SPI)、替米考星(TIL)和泰乐菌素(TYL)]残留检测的HPLC-MS/MS法。样品经乙腈提取,中性氧化铝和正己烷净化后,以选择反应检测模式检测,基质匹配标准工作曲线定量。在1～100 ng·mL-1范围内,7种药物的峰面积与质量浓度的线性关系良好(R2>0.995)。试验选择不同阴性样品为试样,在4μg·kg-1、20μg·kg-1和40μg·kg-1添加水平下的回收率为75.4%～108%,相对标准偏差为0.665%～12.9%。方法的检出限为1μg·kg-1,定量限为4μg·kg-1。该方法简单,灵敏度高,重现性好,可为水产品中7种大环内酯类抗生素残留的检测提供技术支持。

We developed a high performance liquid chromatography tandem mass spectrometric（HPLC-MS/MS） method for determining 7 macrolide antibiotics [oleandomycin（OLD）,erythromycin（ERM）,kitasamycin（KIT）,josamycin（JOS）,spiramycin（SPI）,tilmicosin（TIL） and tylosin（TYL）] in aquatic products.The samples were extracted with acetonitrile and cleaned up by neutral alumina and n-hexane;data acquisition was achieved by applying selected reaction monitoring（SRM）,and quantification analysis was performed with matrix matched standard calibration curves.The standard curves show good linear between the peak areas and concentrations of 7 macrolides in the range of 1~100 ng·mL-1（R2〉0.995）.The average recovery of the drugs fortified in different negative samples at 3 spiked levels of 4 μg·kg-1,20 μg·kg-1 and 40 μg·kg-1 varies from 75.4% to 108%,and the relative standard deviations vary from 0.665% to 12.9%.The detection limit of the drugs in aquatic products is 1 μg·kg-1 and the quantification limit is 4 μg·kg-1.This simple,sensitive and reproducible method can provide technical support for the determination of 7 macrolide antibiotic residues in aquatic products.