QuEChERS-分散固相萃取-液质联用法测定婴幼儿奶粉中9种禁用安眠药

QuEChERS-dispersed Solid Phase Extraction-ultra Performance Liquid Chromatography-tandem Mass Spectrometry for Determination of 9 Kinds of Banned Soporifics in Infant Milk Powder

违法添加安眠药是影响婴幼儿奶粉质量安全的主要风险因子之一,建立了QuEChERS-分散固相萃取-液质联用法快速测定婴幼儿奶粉中9种禁用安眠药的方法。样品采用QuEChERS提取,然后采用增强型脂质去除分散式固相萃取管(EMR-Lipid dSPE)进行净化,多反应监测采集模式(MRM)进行定性和定量检测,外标法定量。结果表明,9种禁用安眠药在各自线性范围内呈良好的线性关系,相关系数(R2)均大于0.9921,检出限在0.05~0.72 ng/g之间,定量限在0.16~2.9 ng/g之间,3个添加水平的回收率在64.1%~107.4%之间,RSD在1.5%~9.4%之间。该方法具有前处理操作简单、结果准确、检出限低、灵敏度高等优点,适用于婴幼儿奶粉中9种禁用安眠药的快速筛查。

Illegal addition of sleeping pills that affecting the quality and safety of infant milk powder is one of the major risk factors.The QuEChERS-dispersed solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry(QuEChERS-dSPE-UPLC-MS/MS)was established for the rapid determination of 9 kinds of banned soporifics in infant milk powder.The sample was extracted with Quick、Easy、Cheap、Effective、Rugged and Safe(QuEChERS),then purified with enhanced matrix removal lipid-dispersed solid phase extraction(EMR-Lipid-dSPE).The multiple reaction monitor(MRM)acquisition mode was used for qualitative and quantitative detection,and external standard method was used for quantitative detection.The analytes showed good linearities in corresponding concentration ranges with their correlation coefficients(R2)greater than 0.9921.The limit of detection was 0.05~0.72 ng/g,the limit of quantitative was 0.16~2.9 ng/g,the spiked recoveries for analytes at three spiked levels were in the range of 64.1%~107.4%,and RSD were 1.5%~9.4%.The matrix removal effect of this method is sufficient,the pretreatment method is simple,reproducible and sensitive,and suitable for the rapid screening of 9 kinds of banned soporifics in infant milk powder.