固相萃取-超高效液相色谱-电喷雾串联质谱法测定食用油脂中3-氯丙醇酯
作者:
作者单位:

(深圳市疾病预防控制中心, 广东 深圳 518055)

作者简介:

刘红河 男 主任技师 研究方向主要为食品中有机污染物研究 E-mail:liuhonghe@sina.com

通讯作者:

中图分类号:

基金项目:

深圳市科技创新委员会知识创新计划基础研究项目(JCYJ20140410170519145)


Simultaneous determination of 3-chloro-1,2-propanediol (3-MCPD) esters residues in foods by solid phase extraction-ultra performance liquid chromatography-electrospray tandem mass spectrometry
Author:
Affiliation:

(Shenzhen Center for Disease Control and Prevention,Guangdong Shenzhen 518055,China)

Fund Project:

  • 摘要
  • |
  • 图/表
  • |
  • 访问统计
  • |
  • 参考文献
  • |
  • 相似文献
  • |
  • 引证文献
  • |
  • 资源附件
  • |
  • 文章评论
    摘要:

    建立固相萃取-超高效液相色谱-串联质谱联用法(SPE-UPLC-MS/MS)同时测定食品中18种3-氯丙醇酯的方法,并对部分市售含油脂食品中氯丙醇酯的含量进行调查。方法 样品用叔丁基甲醚-乙酸乙酯(8∶2,V/V)超声提取;经Sep-Pak Silica硅胶萃取小柱、OASIS HLB固相萃取小柱(预先用甲醇活化)二次净化,以Acquity UPLC BEH C18色谱柱(2.1 mm×150 mm,1.7 μm)分离,以多反应监测模式(MRM)进行监测,内标法定量。结果18种氯丙醇酯在1.0~200.0 μg/L范围内线性关系良好(r为0.999 1~0.999 8)。食用油在0.10、1.0和10.0 mg/kg 3个添加水平范围内的平均回收率为80.2%~98.5%,RSD<8.1%。食用油中18种氯丙醇酯的检出限在1.17~30.1 μg/kg之间,92.0%(46/50)的食用油中检出多种3-氯丙醇酯,含量分别在7.55~5 360 μg/kg之间;75.0%(9/12)的含油脂食品中检出多种3-氯丙醇酯,含量在6.62~1 569.8 μg/kg之间。结论 建立的固相萃取-超高效液相色谱-电喷雾串联质谱联用法同时测定食品中18种3-氯丙醇酯的方法快速简单、准确有效,可以满足各种食用油和含油脂食品中3-氯丙醇酯的检测要求。

    Abstract:

    To establish a sensitive quantitative method for the simultaneous determination of 3-chloro-1,2-propanediol (3-MCPD) esters in foods by ultra performance liquid chromatography coupled with electrospray tandem mass spectrometry (UPLC-MS/MS) with the pretreatment of solid phase extraction, and investigate ten types of 3-MCPD esters residues in some greasy foods from supermarket.Methods About 0.100 0 g oil sample was accurately weighted and dissolved in a mixture of 10 ml tert-butyl methyl ether (MTBE)-ethyl acetate (8∶2, V/V) and spiked with internal standard. After vortex, the analyte of the extraction were purified by a Sep-pak silica cartridge and a OASIS HLB C18 cartridge (preconditioned with methanol) in turn. The sample extract was separated on an acquity BEH C18 column (2.1 mm×150 mm,1.7 μm), identified by electrospray ionization (ESI) in positive mode using multiple reaction monitoring (MRM), and then detected by ultra performance liquid chromatography-tandem mass spectrometry and quantified with internal standards. Results By the quantification of internal standard, the 18 types of 3-MCPD esters were linear in the range of 1.0~200.0 μg/L with correlation coefficient of 0.999 1~ 0.999 8. The detection limit of the method was ranged from 1.17 to 30.1 μg/kg for edible oils. The recovery of spiked samples at three levels (0.10,1.0 and 10.0 mg/kg) was ranged from 80.2%~98.5% (n=7). And the relative standard derivations (RSD) were lower than 8.1%. In 50 edible oils and 12 greasy foods, 3-MCPD esters were detected at the range of 7.55~5 360 μg/kg with a detection rate of 92.0% (46/50), and in 12 greasy foods, 3-MCPD esters was detected at the range of 6.62~ 1 569.8 μg/kg with a detection rate of 75.0% (9/12).Conclusion The method could be used to detect 3-MCPD esters in edible oils and greasy foods.

    参考文献
    相似文献
    引证文献
引用本文

刘红河,陈慧玲,许欣欣,康莉,廖仕成,毛丽莎.固相萃取-超高效液相色谱-电喷雾串联质谱法测定食用油脂中3-氯丙醇酯[J].中国食品卫生杂志,2016,28(3):327-333.

复制
分享
文章指标
  • 点击次数:
  • 下载次数:
  • HTML阅读次数:
  • 引用次数:
历史
  • 收稿日期:2015-10-10
  • 最后修改日期:
  • 录用日期:
  • 在线发布日期: 2016-06-02
  • 出版日期:
文章二维码
《中国食品卫生杂志》邮寄地址与联系方式变更通知
关闭