PRiME HLB固相萃取-高效液相色谱-串联质谱法同时快速测定鸡蛋中48种兽药残留

PRiME HLB Solid-phase Extraction Procedure Combined with High Liquid Chromatography-Tandem Mass Spectrometry for Multi-residue Determination of 48 Veterinary Drugs in Eggs

建立固相萃取-高效液相色谱-串联质谱同时快速测定鸡蛋中48种兽药残留的分析方法。样品采用90%乙腈水溶液提取,用PRiME HLB小柱净化浓缩后用电喷雾离子源,正负离子扫描,多反应监测模式的高效液相色谱-串联质谱法进行检测,以基质匹配曲线外标法定量。正离子采用CAPCELL PAK C18 MGⅢ-H色谱柱,流动相为0.05%甲酸乙腈和0.1%甲酸水;负离子采用ACQUITY UPLC?BEH C18色谱柱,流动相为5 mmol/L乙酸铵和乙腈。结果表明,鸡蛋样品中的48种兽药残留在0.5~50μg/kg浓度范围内线性关系良好,相关系数(r)为0.9952~1.0000。方法检出限为0.01~0.55μg/kg,定量限为0.03~1.83μg/kg,样品回收率在63.3%~111.4%之间,相对标准偏差小于10%(n=3)。本方法操作快速简单,重复性好,灵敏度较高,适用于鸡蛋中48种兽药残留的快速筛查检测。

A rapid method was developed for the simultaneous multi-residue determination of 48 veterinary drugs in eggs by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)with pass-through solid phase extraction(SPE). The samples were extracted with 90% acetonitrile-water mixtures. The extraction cleaned up with an Oasis PRiME HLB SPE cartridges was determined by liquid chromatography-tandem mass spectrometry in positive and negative ionization mode using an electrospray ionization source with the multiple reaction monitoring mode. Quantitative was achieved by an external calibration procedure using matrix-matched standard solutions. The chromatographic separation was achieved on a CAPCELL PAK C18 MGⅢ-H chromatographic column using 0.05%(v/v)formic acid acetonitrile solution and aqueous 0.1%(v/v)formic acid solution gradient as the mobile phase in the positive ion mode;And on a ACQUITY UPLC BEH C18 column using acetonitrile and 5 mmol/L ammonium acetate aqueous solution gradient as the mobile phase in the negative ion mode. The results showed that the linearities of the 48 veterinary drug residues in 0.5~50 μg/kg had the correlation coefficient and the correlation coefficient were from 0.9952 to 1.0000. The limits of detection(LOD)ranged from 0.01 to 0.55 μg/kg and the limits of quantification(LOQ)ranged from 0.03 to 1.83 μg/kg. The recoveries was 63.3%~111.4%,while the relative standard deviations was less than 10%.The proposed method is sensitive,accurate,and efficient. It is applicable for rapid screening and quantification of 48 veterinary drug residues in eggs.