UPLC-MS/MS法测定婴幼儿乳制品中的氟乙酸钠  

Determination of sodium fluoroacetate in infant dairy products by UPLC-MS/MS

作　　者：张文旭[1] 胡雪 高玉杰 张立佳 

机构地区：[1]内蒙古医科大学附属医院,内蒙古呼和浩特010050 [2]内蒙古伊利实业集团股份有限公司,内蒙古呼和浩特010110

出　　处：《中国酿造》2015年第6期150-153,共4页China Brewing

基　　金："十二五"国家科技支撑计划项目(2012BAK17B00)

摘　　要：采用超高效液相色谱-串联质谱法建立了婴幼儿乳制品中氟乙酸钠的检测方法,为相关中毒事件的样本分析提供检测依据.样品经水稀释、乙腈沉淀蛋白、C18固相萃取填料净化后,低温冷冻离心除掉杂质,含0.1％乙酸水溶液和乙腈梯度洗脱,通过ACQUITYUPLC CSH Fluoro-Phenyl色谱柱分离,电喷雾负离子多反应监测模式进行检测.结果表明,该方法在10-1000μg/L范围内线性良好,相关系数R2＞0.99,定量限0.2 mg/kg.不同添加质量浓度的回收率为91.8％-114.9％,相对标准偏差＜10.0％,精密度试验相对标准偏差＜5.0％.该方法操作快速简单、灵敏度和重现性较好,能够用于婴幼儿乳制品中氟乙酸钠的污染排查和相关中毒事件的样品检测.A UPLC-MS/MS method for determination of sodium fluoroacetate in infant dairy products was developed and the analytical method for the relevant food poison accidents was provided. Samples were ultrasonically extracted with water, protein was precipitated by frozen with acetonitrile and the extracted solution was purified by dispersive DSC-C18. The target compound was separated by ACQUITY UPLC CSH Fluoro-Phenyl with a mobile phase of 0.1% acetic acid solution and acetonitrile, and analyzed by a negative electrospray ion multiple reaction monitoring mode. The standard curves were linear in the concentration range of 10-1 000μg/L with correlation coefficients more than 0.99. The quantification limits was 0.2 mg/kg. The recovery values and the relative standard deviation were 91.8%-114.9% and less than 10.0% at different fortification levels. Due to its simplicity, relatively high sensitivity and reproducibility, the method was suitable for the contamination screening and detection of sodium fluoroacetate in infant dairy products from the poisoning accidents.

关 键 词：超高效液相色谱质谱联用法 氟乙酸钠 中毒检测 婴幼儿乳制品 

分 类 号：R917[医药卫生—药物分析学]