PRiME HLB-超高效液相色谱-串联质谱法测定鸡蛋中硝基咪唑类药物残留量

Determination of nitroimidazoles residues in egg by PRiME HLB combined with ultra performance liquid chromatography-tandem mass spectrometry

目的建立高效液相色谱串联质谱法快速检测鸡蛋中硝基咪唑类药物残留量的分析方法。方法以0.1%甲酸乙腈为提取溶剂,加入盐析剂分层后,用Waters Oasis PRiME HLB法净化,用乙腈和0.1%(V:V)甲酸水溶液作为流动相进行梯度洗脱, C18色谱柱分离,在高效液相色谱-串联质谱仪上采用电喷雾正离子扫描模式检测,基质匹配标准曲线外标法定量。结果该方法在0.5~100 ng/mL范围内具有良好线性关系, 10种硝基咪唑类药物相关系数均大于(r^2)>0.99,方法检出限在0.1~0.3μg/kg范围,定量限在0.3~0.5μg/kg范围。3个浓度水平1.0、5.0、10.0μg/kg加标,平均回收率分别为82.5%~119.1%、80.7%~112.3%、80.6%~118.5%,相对标准偏差(relative standard deviation, RSD)为1.2%~9.1%。结论该方法具有快速、简便、准确、灵敏的特点,适用于鸡蛋中硝基咪唑残留量的分析检测,可用于日常大批量快速筛查工作,有效提高日常工作效率。

Objective To establish a rapid method for the determination of nitroimidazole in eggs by high performance liquid chromatography tandem mass spectrometry.Methods The sample was extracted with 0.1%formic acid acetonitrile and separated by adding salting-out agent.The sample solution was purified by Waters Oasis PRiME HLB method,separated by C18chromatogaphic column with gradient elution of acetonitrile and 0.1%(V:V)famic acid solution,and were detected by electro spray positive ion scanning mode with high performance liquid chromatography tandem mass spectrometry(HPLC-MS/MS),and quantified by matrix-matched calibration.Results The good linear relationship was in the range of 0.5-100μg/mL for analyte,and the correlation coefficient square of the 10 kinds of nitroimidazole residues was greater than 0.99.The limits of detection(LODs)for nitroimidazole were 0.1-0.3μg/kg,and limits of quantitation(LOQs)were 0.3-0.5μg/kg.Three kinds of concentrations were labeled 1.0,5.0 and 10.0μg/kg,respectively,the average recoveries were 82.5%-119.1%、80.7%-112.3%、80.6%-118.5%,and the relative standard deviations(RSDs)were 1.2%-9.1%.Conclusion It is such a rapid,simple,accurate and sensitive method that can be used for the determination of nitroimidazole in egg and daily mass rapid scanning to improve daily work efficiency effectively.