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

[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.