超高效液相色谱-串联质谱法同时测定畜禽肉中林可胺类和大环内酯类抗生素及其代谢物残留  

Simultaneous determination of lincosamides,macrolides and their metabolites residues in livestock and poultry meat by UHPLC-MS/MS

作　　者：魏莉莉 程志 丁一 卢兰香 武传香 王骏 薛霞 刘艳明 WEI Lili;CHENG Zhi;DING Yi;LU Lanxiang;WU Chuanxiang;WANG Jun;XUE Xia;LIU Yanming(Shandong Institute for Food and Drug Control,Key Laboratory of Supervising Technology for Meat and Meat Products for State Market Regulation,Shandong Research Center of Engineering and Technology for Safety Inspection of Food and Drug,Jinan 250101,China)

机构地区：[1]山东省食品药品检验研究院,国家市场监督重点实验室(肉及肉制品监管技术),产业技术基础公共服务平台,济南250101

出　　处：《分析试验室》2024年第7期1017-1023,共7页Chinese Journal of Analysis Laboratory

摘　　要：建立了畜禽肉中林可胺类(林可霉素、吡唎霉素)、大环内酯类抗生素(螺旋霉素、替米考星、竹桃霉素、红霉素、泰乐菌素、吉他霉素、克拉霉素、罗红霉素、交沙霉素、泰万菌素)及其2种代谢物(新螺旋霉素、3-O-乙酰泰乐菌素)残留量的超高效液相色谱-串联质谱(UHPLC-MS/MS)分析方法。试样采用70%(V/V)乙腈水超声提取,磷酸盐缓冲溶液(pH 9.0)稀释,C18固相萃取柱净化;采用BEH C18色谱柱(100 mm×2.1 mm,1.7μm)分离,以乙腈和0.1%甲酸水为流动相梯度洗脱;采用电喷雾串联质谱仪,在多离子反应监测(MRM)模式下,外标法定量。结果表明,14种药物在0.25~50.0 ng/mL范围内线性关系良好(r>0.999),定量限(LOQ)为1.0μg/kg。在1,10,100μg/kg加标水平下,不同基质中平均回收率为76.6%~111.5%,相对标准偏差小于13%,满足兽药残留实验室质量控制规范要求,可实现GB 31650-2019中涵盖的林可胺类、大环内酯类及其代谢物的同时测定。An ultra high performance liquid chromatography-tandem mass spectrometry method was established for the determination of lincosamides(lincomycin and pirlimycin),macrolides(spiramycin,tilmicosin,oleandomycin,erythromycin,tylosin,kitamycin,clarithromycin,roxithromycin,josamycin,tylvalosin)and two metabolites(neospiramycin and 3-O-acetyltylosin)in livestock and poultry meat.The samples were ultrasonically extracted with 70%acetonitrile solution,diluted with phosphate buffer solutions(pH 9.0),and then purified with C18 solid phase extraction columns.The extracts were separated on a reversed-phase mode BEH C18(100 mm×2.1mm,1.7μm)chromatographic column by gradient elution with acetonitrile and 0.1%formic acid aqueous solution.Tandem mass spectrometry with electrospray ionization was used to carry out quantitative analysis in positive ion and multiple reaction monitoring(MRM)mode by external standard method.The results showed that good linearities were obtained in the range of 0.25-50 ng/mL with the correlation coefficients higher than 0.999.The limits of quantification(LOQs)were 1.0μg/kg for target analytes.At three spiked levels of 1,10 and 100μg/kg,the mean recoveries for 14 target compounds were from 76.6%to 111.5%,and the relative standard deviations were less than 13%.The precision and accuracy of this method can meet criterion on quality control for residue analysis of veterinary drugs.The developed method can be applied to the simultaneous detection of lincosamides,macrolides and their metabolites.

关 键 词：林可胺类抗生素 大环内酯类抗生素 代谢物 超高效液相色谱-串联质谱 固相萃取 

分 类 号：O657.63[理学—分析化学]