通过式固相萃取-超高效液相色谱串联质谱法同时测定猪肝中19种磺胺类兽药残留  

Simultaneous Determination of 19 Sulfonamides Drugs Residues in Pig Liver by Pass-Though Solid Phase Extraction Coupled with Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：王展华 王一涵 施贝 张文萍 朱蕾颖 张翀宇 WANG Zhan-hua;WANG Yi-han;SHI Bei(Key Laboratory of Functional Food Nutrition and Quality Safety for State Market Regulation,Key Laboratory of Health Food Quality Safety of Provincial Market Regulation,Zhejiang Institute of Food and Drug Control,Hangzhou,Zhejiang 310052)

机构地区：[1]国家市场监管重点实验室(功能食品质量与安全领域),浙江省市场局重点实验室(保健品质量安全重点实验室),浙江省食品药品检验研究院,浙江杭州310052

出　　处：《安徽农业科学》2022年第18期159-164,共6页Journal of Anhui Agricultural Sciences

基　　金：浙江省基础公益研究计划(LGC20C200001)。

摘　　要：[目的]建立一种通过式固相萃取柱净化-超高效液相色谱串联质谱法测定猪肝中19种磺胺类药物残留的分析方法。[方法]样品均质后,使用80%的乙腈水溶液超声提取10 min,使用ProElut PLS-A固相萃取柱进行净化,使用BEH C_(18)色谱柱进行分离,以0.1%的甲酸水和0.1%甲酸乙腈甲醇混合液(1+1)为流动相按比例进行梯度洗脱,使用正离子模式。采用质谱多重反应监测模式(MRM),采用空白基质绘制标准曲线定量。[结果]19种磺胺类药物在2~80μg/L呈现良好的线性关系(R^(2)>0.99),方法检出限为0.1~1.4μg/kg,定量限为0.3~4.7μg/kg,方法的回收率为74.8%~123.2%,精密度相对标准偏差(RSD)<5%。[结论]该方法操作流程简便、结果准确可靠,可应用于猪肝中磺胺类药物残留的检验检测方法。[Objective]To establish an analytical method for the determination of 19 kinds of sulfonamides residues in pig liver by solid-phase extraction column clean up-ultra performance liquid chromatography-tandem mass spectrometry.[Method]After the sample was homogenized,it was ultrasonically extracted with 80%acetonitrile aqueous solution for 10 min,purified with ProElut PLS-A solid phase extraction column,and separated with BEH C_(18) chromatographic column.0.1%formic acid water and 0.1%formic acid acetonitrile methanol mixture(1+1)were used as mobile phases for gradient elution.Positive ion mode and mass spectrometry multiple response monitoring mode(MRM)was used for determination.External standard method was used for quantification.[Result]The 19 sulfonamides showed a good linear relationship at 2-80μg/L(R^(2)>0.99),the detection limit of the method was 0.1-1.4μg/kg,and the quantification limit was 0.3-4.7μg/kg.The recovery rate of the method was 74.8%-123.2%,precision relative standard deviation(RSD)<5%.[Conclusion]The method is simple,accurate and reliable,and can be used for the detection of sulfonamides drug residues in pig liver.

关 键 词：固相萃取 超高效液相色谱串联质谱法 磺胺类药物 兽药残留 猪肝 

分 类 号：S859.84[农业科学—临床兽医学]