全自动样品处理平台在食用油脂中氯丙醇酯和缩水甘油酯测定的应用研究
作者:
作者单位:

1.福建中医药大学药学院,福建 福州 350122;2.福建省人兽共患病研究重点实验室,福建省疾病预防控制中心,福建 福州 350001;3.福建农林大学食品科学学院,福建 福州 350000;4.福建医科大学公共卫生学院,福建 福州 350108;5.福州国际旅行卫生保健中心,福建 福州 350003

作者简介:

蓝丽华 女 在读研究生 研究方向为药物分析 E-mail: 951815806@qq.com

通讯作者:

傅武胜 男 主任技师 研究方向为食品化学污染物的检测技术和风险评估 E-mail: fwsfqm@126.com

中图分类号:

R155

基金项目:

国家自然基金(81172671);福建省科技创新平台建设项目(2019Y2001);福建省卫生系统中青年骨干人才培养项目(2013-ZQN-ZD-9);福建省杰出青年基金(2011J06011)


Application of fully automated sample processing platform for the determination of chloropropanol esters and glycidyl esters in edible fats and oils
Author:
Affiliation:

1.College of Pharmacy, Fujian University of Traditional Chinese Medicine, Fujian Fuzhou 350122, China;2.Fujian Key Laboratory of Zoonoses, Fujian Provincial Center for Disease Control and Prevention, Fujian Fuzhou 350001, China;3.College of Food Science, Fujian Agriculture and Forestry University, Fujian Fuzhou 350000, China;4.School of Public Health, Fujian Medical University, Fujian Fuzhou 350108, China;5.Fuzhou International Travel Healthcare Center, Fujian Fuzhou 350003, China

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    摘要:

    目的 建立一种在线全自动快速测定食用油脂中氯丙醇酯(MCPDE)和缩水甘油酯(GE)含量的分析方法,并考察植物油种类、温度等因素对GE转化为3-氯-1,2-丙二醇(3-MCPD)的影响。方法 参考AOCS Cd 29c-13基本原理,将样品置于全自动样品前处理平台进行水解、氯代、液-液萃取和衍生,采用毛细管柱(DB-5MS柱)分离,多反应监测模式(MRM)采集,内标法定量。结果 5种植物油中GE的转化率差异不明显,但温度的影响略大,当10 ℃下水解7 min时,MCPDE和GE水解基本完成。3-氯-1,2-丙二醇酯(3-MCPDE)、2-氯-1,3-丙二醇二酯(2-MCPDE)和GE的检出限均为5 μg/kg(以醇计),在0~0.4 μg/mL范围内浓度与峰面积比值呈良好的线性关系(决定系数R2≥0.999);在20~2 500 μg/kg范围内加标,MCPDE和GE的回收率范围为90.3%~109.7%,相对标准偏差(n=6)为1.3%~7.7%,精密度上全自动方法优于手工前处理操作。与食品安全国家标准方法(送审稿)进行对比,方法间结果具有可比性,将该方法用于FAPAS考核样的测定,结果满足要求。结论 全自动法操作简便,灵敏度较高,大大降低了人工操作的劳动强度,提高了检测效率和结果的重复性,较好满足了食用油脂中MCPDE和GE的定量测定。

    Abstract:

    Objective An online fully automated alkaline hydrolysis method for the determination of chloropropanol esters (MCPDE) and glycidyl esters (GE) in edible oils and fats was developed, and the effects of vegetable oil type and temperature on the conversion of GE to 3-chloro-1,2-propanediol (3-MCPD) were investigated.Methods Based on the basic principles of AOCS Cd 29c-13, the samples were subjected to hydrolysis, chlorination, liquid-liquid extraction and derivatization on a fully automated sample pretreatment platform, and then separated by a DB-5MS column after injection. The data was determined by multiple reaction monitoring mode (MRM) coupled with the internal standard method.Results The efficiency of GE conversion to 3-MCPDE in the five vegetable oils was significant different. However, the effect of temperature was relatively greater. The alkali hydrolysis time was optimized, and the hydrolysis of MCPDE and GE was basically completed when the hydrolysis was carried out for 7 min at 10℃. The limits of detection for 2-chloro-1,3-propanediol (2-MCPDE), 3-chloro-1,2-propanediol (3-MCPDE) and GE were all 5 μg/kg calculated by their free forms. There was a good linear relationship between the concentration and ratio of the response ranged from 0 to 0.4 μg/mL. When spiked from 20 to 2 500 μg/kg, the recoveries of MCPDE and GE ranged from 90.3% to 109.7% with the relative standard deviation (n=6) of 1.3%-7.7%, indicating that the precision was better than that of the manual procedure. The method was comparable with the Chinese national standard method for food safety under reviewed and was successfully applied to the determination of FAPAS proficiency test samples.Conclusion The novel automatic procedure has the advantages of simple operation and high sensitivity, which reduces the labor intensity, improves the detection efficiency and repeatability compared with the reported manual procedure, and can better meet the requirement for quantification of MCPDE and GE in edible oils and fats.

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蓝丽华,林丽珊,傅武胜,陈丹,叶洪,桂荣娟.全自动样品处理平台在食用油脂中氯丙醇酯和缩水甘油酯测定的应用研究[J].中国食品卫生杂志,2022,34(3):531-538.

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  • 收稿日期:2021-12-14
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  • 在线发布日期: 2022-07-07
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