摘要
建立了畜禽产品中维吉尼亚霉素M1和S1药物残留检测的液相色谱-串联质谱分析方法。样品以甲醇-乙腈溶液(1∶1,v/v)提取,上清液经0.01 mol/L磷酸二氢铵溶液稀释后,Oasis HLB固相萃取小柱净化,Luna C18色谱柱分离,以乙腈和含0.1%(体积分数)甲酸的5 mmol/L乙酸铵水溶液作为流动相进行梯度洗脱,电喷雾正离子模式电离(ESI+),多反应监测(MRM)模式检测,外标法定量。该方法对两物质线性范围均为0.15～10.0μg/L,相关系数r2均大于0.999;定量下限均为0.25μg/kg。在不同基质中,0.25、0.50、2.5μg/kg 3个添加水平的平均回收率范围为71.2%～98.4%,精密度范围为3.6%～15.4%。该方法具有快速简便、灵敏度高、准确性强等特点,适用于畜禽产品中维吉尼亚霉素的检测。
A liquid chromatography-tandem mass spectrometry method was established for the determination of virginiamycin M1 and S1 residues in livestock and poultry products.The sample was extracted by methanol-acetonitrile solution（1∶1,v/v）.The supernatant was diluted with 0.01 mol/L ammonium dihydrogen phosphate solution,then purified and concentrated on an Oasis HLB cartridge.The separation of virginiamycin M1 and S1 was performed on a Luna C18 column with the mobile phases acetonitrile and 5 mmol/L ammonium acetate aqueous solution（containing 0.1%（v/v） formic acid） in a gradient elution mode.The identification and quantification of the drugs were carried out by positive electrospray ionization（ESI＋） in the multiple reaction monitoring（MRM） mode using external standard method.The calibration curves showed good linearity in the range of 0.15-10.0 μg/L with correlation coefficients（r2） above 0.999.The limits of quantities（LOQs） were both 0.25 μg/kg.The average recoveries of the two drugs spiked at 0.25,0.5 and 2.5 μg/kg levels in different matrices were between 71.2% and 98.4%,and the relative standard deviations（RSDs） were between 3.6% and 15.4%.The method is simple,rapid,sensitive and accurate.It is suitable for the confirmation and quantification of virginiamycin M1 and S1 residues in livestock and poultry products.
出处
《色谱》
CAS
CSCD
北大核心
2012年第5期463-467,共5页
Chinese Journal of Chromatography
基金
福建省科技攻关重点项目(2010Y0001)
国家质检总局科研项目(2009IK143)
