超高效液相色谱-串联质谱法测定鹅可食用组织中维吉尼亚霉素M_(1)的残留量

Determination of Virginiamycin M_(1) Residues in Goose Tissues by Ultra-Performance Liquid Chromatography Tandem Mass Spectrometry

本研究建立了超高效液相-串联质谱法(UPLC-MS/MS)检测鹅肌肉、肝脏、肾脏、皮脂组织中维吉尼亚霉素M_(1)的残留检测方法。组织样品使用乙腈提取、正己烷脱脂,经过滤后直接运用超高效液相色谱-串联质谱检测,外标法定量,采用电喷雾离子源(ESI^(+)),选择多反应监测(MRM)模式进行分析。结果表明:鹅各组织的定量限分别为肌肉10.0μg/kg、肝脏50.0μg/kg、肾脏50.0μg/kg、皮脂50.0μg/kg,平均回收率分别为肌肉93.09%~98.62%、肝脏98.41%~103.8%、肾脏101.5%~113.3%、皮脂100.9%~114.3%。批内、批间的RSDs均符合相关要求。该方法简化了样品前处理过程,具有较好的灵敏度、准确性,可用于检测鹅可食用组织中维吉尼亚霉素M1的残留量。

A reliable UPLC-MS/MS method with high sensitivity was developed and validated for the determination of virginiamycin M_(1) in muscle,fat,liver and kidney samples of geese.Virginiamycin M_(1) was extracted using acetonitrile and extracts were defatted by N-hexane.The virginiamycin M_(1) extracts were fi ltered and quantifi ed by UPLC-MS/MS method.An electrospray ion source(ESI^(+))was used and multiple reaction monitoring(MRM)mode was selected for analysis.The results showed that the detection limits were 10.0μg/kg for muscles,50.0μg/kg for livers,50.0μg/kg for kidneys and 50.0μg/kg for sebums.The average recoveries were 93.09%-98.62%of muscles,98.41%-103.8%of livers,101.5%-113.3%of kidneys and 100.9%-114.3%of sebums.RSDS within and between batches all met the relevant requirements.This method simplifi ed the process of sample treatment and had good sensitivity and accuracy.Therefore,it was suitable for the detection and quantifi cation of virginiamycin M_(1) residues in livestock and poultry products.