Rapid and automated analysis of aflatoxin M1 in milk and dairy products by online solid phase extraction coupled to ultra-high-pressure-liquid-chromatography tandem mass spectrometry
Rapid and automated analysis of aflatoxin M1 in milk and dairy products by online solid phase extraction coupled to ultra-high-pressure-liquid-chromatography tandem mass spectrometry
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DOI：
10.1016/j.chroma.2015.10.094
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发表时间：
2016-01-08
影响因子：
4.1
通讯作者：
Rastrelli, Luca
中科院分区：
文献类型：
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作者：
Campone, Luca;Piccinelli, Anna Lisa;Rastrelli, Luca
本研究报告了一种快速、自动化的分析方法，用于分析牛奶和乳制品中的黄曲霉毒素M1(AFM1)。该方法基于蛋白质沉淀和AFM1的同时提取，通过盐诱导液液萃取(SI-LLE)，然后在线固相萃取(Online SPE)与超高压-液-质联用(UHPLC-MS/MS)分析相结合，实现了AFM1的自动预浓缩、净化和灵敏、选择性的测定。详细研究了影响分析方法提取效率和准确度的主要参数。在最佳条件下，乙腈为提取变性剂，氯化钠为盐析剂。离心后，有机相(乙腈)用水(1：9v/v)稀释，用在线C18小柱与UHPLC柱联用纯化1mL。最后，将选择性反应监测(SRM)采集模式应用于AFM1的检测，并对不同的乳制品(全脂和脱脂牛奶、酸奶、山羊奶和婴儿配方奶粉)进行了验证研究，提供了低于欧盟第1881/2006号法规允许的人类直接食用牛奶和乳制品中AFM1最高限量约25倍的方法定量限。回收率(86%-102%)和重复性(RSD
This study reports a fast and automated analytical procedure for the analysis of aflatoxin M1 (AFM1) in milk and dairy products. The method is based on the simultaneous protein precipitation and AFM1 extraction, by salt-induced liquid-liquid extraction (SI-LLE), followed by an online solid-phase extraction (online SPE) coupled to ultra-high-pressure-liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) analysis to the automatic pre-concentration, clean up and sensitive and selective determination of AFM1. The main parameters affecting the extraction efficiency and accuracy of the analytical method were studied in detail. In the optimal conditions, acetonitrile and NaCl were used as extraction/denaturant solvent and salting-out agent in SI-LLE, respectively. After centrifugation, the organic phase (acetonitrile) was diluted with water (1:9 v/v) and purified (1 mL) by online C18 cartridge coupled with an UHPLC column. Finally, selected reaction monitoring (SRM) acquisition mode was applied to the detection of AFM1.Validation studies were carried out on different dairy products (whole and skimmed cow milk, yogurt, goat milk, and powder infant formula), providing method quantification limits about 25 times lower than AFM1 maximum levels permitted by EU regulation 1881/2006 in milk and dairy products for direct human consumption. Recoveries (86-102%) and repeatability (RSD