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固相萃取净化/高效液相色谱-串联质谱法测定饲料中7种大环内酯类药物含量
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作者单位
龚兰,栾枫婷,温天锐,陈明,邓博文,张泽璟,魏瑞成,王冉 江苏省农业科学院农产品质量安全与营养研究所省部共建国家重点实验室培育基地-江苏省食品质量安全重点实验室 
基金项目:农业部农业行业标准项目资助(028042911625)
中文摘要:建立了添加剂预混合饲料、精料补充饲料、配合饲料和浓缩饲料中7种大环内酯类药物(替米考星、罗红霉素、螺旋霉素、泰乐菌素、红霉素、克拉霉素和阿奇霉素)含量的高效液相色谱-串联质谱(HPLC-MS/MS)测定方法。饲料样品经1%氨化乙腈提取,Oasis PRiME HLB固相萃取柱净化后,采用ACQUITY UPLC BEH C18色谱柱(2.1 mm×100 mm,1.7 μm)分离,以0.1%甲酸水-乙腈为流动相梯度洗脱,电喷雾离子源正离子模式下检测,外标法定量。结果表明,替米考星、螺旋霉素和红霉素的线性范围为0.5~50 μg/L(r2>0.99),罗红霉素、泰乐菌素、克拉霉素和阿奇霉素的线性范围为0.25~50 μg/L(r2>099);7种待测物的检出限(LOD)为1.25~2.5 μg/kg,定量下限为2.5~5.0 μg/kg,5、10、50 μg/kg 3个加标浓度下的平均回收率为61.4%~103%,批内和批间相对标准偏差为0.43%~15%。该方法简便、快速、灵敏,基质干扰小,适用于各类饲料中大环内酯类药物的常规监测和定量测定。
中文关键词:大环内酯类药物  饲料  高效液相色谱-串联质谱  固相萃取
 
Analysis of Macrolide Antibiotics in Feeds by High Performance Liquid Chromatography-Tandem Mass Spectrometry Based on Solid Phase Extraction
Abstract:A high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) was developed for the simultaneous determination of seven macrolide antibiotics,ie.tilmicosin,roxithromycin,spiramycin,tylosin,erythromycin,clarithromycin and azithromycin in additive premix,concentrate supplement,complete feed and concentrated feed.The samples were extracted with 1% ammoniated acetonitrile solution,followed by Oasis PRiME HLB solid phase extraction for further purification.The analytes were separated on an ACQUITY UPLC BEH C18 column(2.1 mm×100 mm,1.7 μm) by gradient elution using 0.1% formic acid solution and acetonitrile as mobile phases,then analyzd by MS/MS with electrospray ionization in positive mode,and quantified by external standard method.Results showed that there were good linear relationships for 3 target analytes,ie.tilmicosin,spiramycin and erythromycin in the concentration range of 0.5-50 μg/L(r2>0.99) and for the other 4 target analytes in the range of 0.25-50 μg/L(r2>0.99).The limits of detection and the limits of quantitation were in the ranges of 1.25-2.5 μg/kg and 2.5-5.0 μg/kg,respectively.At three spiked levels of 5,10 and 50 μg/kg,the average recoveries for target compounds ranged from 61.4% to 103% with relative standard deviations of 0.43%-15%.The developed method is simple,rapid,sensitive and low matrix interference,and it is suitable for the routine supervision and quantitative detection of macrolide antibiotics in different feeds.
Key Words:macrolide antibiotics  feed  high performance liquid chromatography-tandem mass spectrometry  solid phase extraction
引用本文:龚兰,栾枫婷,温天锐,陈明,邓博文,张泽璟,魏瑞成,王冉.固相萃取净化/高效液相色谱-串联质谱法测定饲料中7种大环内酯类药物含量[J].分析测试学报,2020,39(7):874-880.
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