一步式QuEChERS结合超高效液相色谱-串联质谱快速测定风干牦牛肉中20种真菌毒素  

Rapid Determination of Twenty Mycotoxins in Air-Dried Yak Meat by One-Step QuEChERS Combined with Ultra-Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：夏寒 谢瑜杰 严晓贤 仝凯旋 常巧英[1] 范春林[1] 朱浙辉 陈辉[1] XIA Han;XIE Yujie;YAN Xiaoxian;TONG Kaixuan;CHANG Qiaoying;FAN Chunlin;ZHU Zhehui;CHEN Hui(Chinese Academy of Inspection and Quarantine,Beijing 100176,China;College of Chemistry and Materials Science,Hebei University,Baoding 071002,China;Tibet Product Quality Supervision and Inspection Institute,Lhasa 850000,China)

机构地区：[1]中国检验检疫科学研究院,北京100176 [2]河北大学化学与材料科学学院,河北保定071002 [3]西藏自治区产品质量监督检验所,西藏拉萨850000

出　　处：《食品科技》2025年第1期337-346,共10页Food Science and Technology

基　　金：中国检科院基本科研业务费项目(2023JK001)。

摘　　要：文章建立了一步式Qu ECh ERS结合超高效液相色谱-串联质谱(Ultra-high performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)同时测定风干牦牛肉中20种真菌毒素的分析方法。样品水化后,经3%酸化乙腈提取,加入4 g MgSO_(4)和1 g NaCl盐析,经过十八烷基硅烷和N-丙基乙二胺填料净化,采用ACQUITY BEH C_(18)色谱柱分离,以0.1%甲酸水溶液(含2mmol/L甲酸铵)-甲醇为流动相,在多重反应监测模式下进行测定,外标法定量。结果表明,20种真菌毒素在0.05~200μg/L范围内线性关系良好,相关系数(R^(2))≥0.9915;检出限为0.075~0.400μg/kg,定量限为0.125~1.250μg/kg;1倍、2倍和10倍定量限3个添加水平的平均回收率为74.2%~110.4%;相对标准偏差为0.8%~9.0%。该方法采用新型一步式QuEChERS结合UPLCMS/MS,实现了前处理自动化,操作简单、减少人为操作步骤、提高试验效率,适用于风干牦牛肉中20种真菌毒素的快速测定,为肉制品中真菌毒素的测定提供方法支持。A method was developed for the simultaneous determination of twenty mycotoxins in air-dried yak meat using one-step QuEChERS combined with ultra-high performance liquid chromatographytandem mass spectrometry(UPLC-MS/MS).After sample hydration,the sample was extracted with 3%acidified acetonitrile,followed by salt partitioning with 4 g of MgSO4 and 1 g of NaCl.The extract was purified using octadecylsilane(C_(18))and primary secondary amine(PSA)solid-phase extraction.Separation was performed on an ACQUITY BEH C18 column,with a mobile phase consisting of 0.1%formic acid aqueous solution(containing 2 mmol/L ammonium formate)and methanol.Detection was carried out under multiple reaction monitoring(MRM)mode,with quantification by the external standard method.The results showed that the twenty mycotoxins exhibited good linearity in the range of 0.05μg/L to 200μg/L,with correlation coefficients(R^(2))≥0.9915.The limits of detection(LODs)ranged from 0.075μg/kg to 0.400μg/kg,and the limits of quantification(LOQs)ranged from 0.125μg/kg to 1.250μg/kg.The average recovery rates at three spiking levels(1×,2×,and 10×LOQ)ranged from 74.2%to 110.4%,with relative standard deviations(RSDs)ranging from 0.8%to 9.0%.This method,which integrates the novel one-step QuEChERS procedure with UPLC-MS/MS,automates the sample preparation process.It is simple to operate,reduces manual steps,and improves experimental efficiency,making it suitable for the rapid determination of twenty mycotoxins in air-dried yak meat and providing methodological support for mycotoxin testing in meat products.

关 键 词：超高效液相色谱-串联质谱 真菌毒素 风干牦牛肉 一步式QuEChERS 

分 类 号：TS207.4[轻工技术与工程—食品科学]