高效液相色谱-串联质谱法测定牛可食性组织中红霉素的残留

目的：建立测定牛可食性组织中红霉素残留的高效液相色谱-串联质谱法（LC-MS/MS），为动物性食品中牛可食性组织残留的监督检验和残留监控提供技术支持。方法：用乙腈提取，正己烷除脂离心后用0.22 μm的有机针孔滤膜过滤，采用日本资生堂CAPCELL PAK MGⅡ-C₁₈（4.6 mm×150 mm，5 μm）色谱柱。流动相为乙腈-0.5%氨水（92：8），流速为0.5 mL·min^-1，柱温为30℃，进样量为5 μL，采用电喷雾离子源ESI，正离子模式，选择MRM多反应监测等质谱条件进行样品检测。结果：红霉素的保留时间为5.967 min，峰形良好、无杂峰干扰，并在5~200 ng·mL^-1浓度范围内线性关系良好（r²=0.990 0，n=5）。低、中、高3个浓度的平均回收率在84.6%~107.6%之间，批内精密度<9%，批间精密度<10%，检测下限为5 μg·kg^-1，定量下限为20 μg·kg^-1，符合检测要求。结论：本文建立的LC-MS/MS检测方法灵敏度高、稳定性好，可用于检测牛可食性组织中的红霉素。

Objective: To establish an high performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for determination of erythromycin residues in bovine edible tissue to provide technical support for the supervision and monitoring of erythromycin residues in animal food. Methods: First,samples were extracted with acetonitrile,centrifuged after being degreased with n-hexane,and then filtered through a 0.22 μm organic pinhole filter. The separation was peformed on CAPCELL PAK MGII-C₁₈ column (4.6 mm×150 mm, 5 μm) with acetonitrile-0.5% ammonia water (92:8) as the mobile phase at flow rate of 0.5 mL·min^-1. The column temperature was 30and the sampling volumn was 5 μL. The samples were detected by using electrospray ion source ESI under positive ion scanning mode,MRM multi-reaction monitoring and other mass spectrometry conditions. The electrospray was operated with the source ESI under positive ionization scanning mode and the drug was identified under multiple reaction monitoring (MRM) mode. Samples were detected under mass spectrometry conditions such as all above. Results: The retention time of erythromycin was 5.967 min,with a good chromatographic peak shape which got a good seperation from disturbance peaks and a good linear relationship within the concentration range of 5-200 ng·mL^-1 (r²=0.990 0,n=5). The relative recoveries of low,medium and high concentrations ranged from 84.6% to 107.6%,the intra-day precisions were<9%,the inter-day precisions were <10%,the limit of detection (LOD) of the method was 5 μg·kg^-1 and the limit of quantitation (LOQ) was 20 μg·kg^-1,which met the test requirements. Conclusion: The LC-MS/MS method established in this study has high sensitivity and stability,and can be used to detect erythromycin in bovine edible tissue.

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