双柱净化-高效液相色谱-串联质谱法测定猪肉中7种头孢菌素残留量

Determination of Seven Cephalosporin Residues in Pork with Dual Solid-Phase Extraction Coupled with High Performance Liquid Chromatography-Tandem Mass Spectrometry

建立了猪肉中7种头孢菌素类药物残留量的双柱净化-高效液相色谱-串联质谱检测方法。样品经85%乙腈水溶液提取,正己烷除脂,HLB及MAX双固相萃取小柱净化,以0.1%甲酸水溶液和乙腈为流动相,反相C_(18)色谱柱梯度洗脱分离,采用电喷雾电离正离子源(ESI+),以多反应监测(MRM)模式进行检测。7种化合物在2-100 ng/mL范围内呈良好的线性关系,相关系数(r^(2))大于0.99。在5-20μg/kg添加范围内,平均回收率为80.7%-112%,相对标准偏差为2.5%-8.6%。方法检出限为0.08-0.2μg/kg,定量限为0.2-0.6μg/kg。建立的方法灵敏度高、准确性好,适用于猪肉中头孢菌素类药物残留的检测。

A method for the determination of seven cephalosporin residues in pork by high performance liquid chromatography-mass spectrometry coupled with dual solid-phase extraction was established.The samples were extracted with 85% acetonitrile aqueous solution, defatted by n-hexane, and purified by HLB and MAX SPE column.The analytes were separated on a C_(18) reversed-phase column with 0.1% formic acid aqueous solution and acetonitrile as mobile phases, and finally analyzed using electrospray ionization in positive ion mode(ESI^(+)) with multiple reaction monitoring(MRM).The results showed good linearity in the range of 2-100 ng/mL,and the correlation coefficients( r^(2)) were more than 0.99.The average recoveries and relative standard deviation were 80.7%-112% and 2.5%-8.6%,respectively in the spiked ranges of 5-20 μg/kg.The limits of detection and the limits of quantification were 0.08-0.2 μg/kg and 0.2-0.6 μg/kg, respectively for seven cephalosporins.The method is sensitive and accurate, and suitable for the detection of cephalosporins in pork.