改进QuEChERS净化液相色谱串联质谱测定海参及制品中外源糖类物质  

Determination of Exogenous Carbohydrates in Sea Cucumber and Its Products by Modified QuEChERS Purification and Liquid Chromatography-Tandem Mass Spectrometry

作　　者：程志 魏莉莉 宿书芳 刘艳明 薛霞 胡梅 万宇平 吴小胜 CHENG Zhi;WEI Lili;SU Shufang;LIU Yanming;XUE Xia;HU Mei;WAN Yuping;WU Xiaosheng(Shandong Institute for Food and Drug Control,Key Laboratory of Supervising Technology for Meat and Meat Products for State Market Regulation,Industrial Technology Foundation Public Service Platform,Jinan 250101,China;Beijing Qinbang Technology Co.,Ltd.,Beijing 102200,China)

机构地区：[1]山东省食品药品检验研究院(国家市场监督重点实验室(肉及肉制品监管技术)(产业技术基础公共服务平台)),山东济南250101 [2]北京勤邦生物技术有限公司,北京102200

出　　处：《食品科技》2025年第2期318-325,共8页Food Science and Technology

基　　金：国家市场监督管理总局科技计划项目(2022MK072)。

摘　　要：文章建立了一种QuEChERS净化液相色谱-串联质谱测定海参及制品中外源糖类物质的方法。实验使用乙醇-水作为提取溶剂,提取液放入内含C18填料和增强型脂质去除净化剂(QuEChERS dSPE EMR-Lipid,EMR)的净化管中快速净化。采用大气压化学离子源(Atmospheric pressure chemical ionization,APCI)负离子模式,多反应监测模式(Multiple reaction monitoring,MRM)对海参和海参产品的外源糖类物质种类进行快速分析,并使用外标法定量。在10.0~750 mg/L浓度区间内,5种目标物都存在着较强的二次方拟合相关性,相关系数均大于0.999。方法检出限为40~80 mg/kg,方法定量限为100~200 mg/kg。目标物回收率为83.1%~103.2%,相对标准偏差不超过8.70%。预处理过程简便、提取效率高、净化效果显著,而且检测限低,可以迅速、准确地对海参和其产品进行分析。A method for the determination of exogenous carbohydrates in sea cucumbers and their products was developed using QuEChERS purification and liquid chromatography-tandem mass spectrometry.Ethanol-water was used as the extraction solvent,and the extract was quickly purified by placing it into a purification tube containing C_(18)packing and an enhanced lipid-removal agent(QuEChERS dSPE EMR-Lipid,EMR).Atmospheric Pressure Chemical Ionization(APCI)in negative ion mode and multiple reaction monitoring(MRM)were employed to rapidly analyze the types of exogenous carbohydrates in sea cucumbers and their products,and quantification was performed using the external standard method.Over the concentration range of 10.0 mg/L to 750 mg/L,the five target compounds exhibited strong quadratic fitting correlations,with correlation coefficients greater than 0.999.The limits of detection of the method were between 40 mg/kg and 80 mg/kg,and the limit of quantification were between 100 mg/kg and 200 mg/kg.The recovery of target compounds ranged from 83.1%to 103.2%,with relative standard deviation values not exceeding 8.70%.The method features simple pre-processing,high extraction efficiency,significant purification effects,and low detection limits,enabling rapid and accurate analysis of sea cucumbers and their products.

关 键 词：外源性糖 海参及其制品 QUECHERS 超高效液相色谱-串联质谱法 

分 类 号：TS207.3[轻工技术与工程—食品科学]