色谱 ›› 2019, Vol. 37 ›› Issue (10): 1048-1052.DOI: 10.3724/SP.J.1123.2019.03016

• 特别策划:固相萃取和QuEChERS应用专栏 • 上一篇    下一篇

分散固相萃取结合气相色谱-高分辨质谱快速筛查酱油中多种氯丙醇

黄超群, 陈钦可, 陈丽, 王云宇, 马喆, 沈咪, 黄佳波   

  1. 浙江省检验检疫科学技术研究院, 浙江 杭州 310016
  • 收稿日期:2019-03-14 出版日期:2019-10-08 发布日期:2020-12-11
  • 通讯作者: 黄超群,Tel:(0571)81100300,E-mail:huangchaoqun18@163.com.

Determination of multiple chloropropanols in soy sauce by dispersive solid phase extraction-gas chromatography-high resolution mass spectrometry

HUANG Chaoqun, CHEN Qinke, CHEN Li, WANG Yunyu, MA Zhe, SHEN Mi, HUANG Jiabo   

  1. Zhejiang Academy of Science and Technology for Inspection and Quarantine, Hangzhou 310016, China
  • Received:2019-03-14 Online:2019-10-08 Published:2020-12-11

摘要: 建立了酱油中1,3-二氯-2-丙醇、2,3-二氯-1-丙醇、3-氯-1,2-丙二醇和2-氯-1,3-丙二醇的分散固相萃取-气相色谱-高分辨质谱快速筛查检测方法。样品采用乙酸乙酯提取,提取液浓缩后经N-丙基乙二胺净化,气相色谱-高分辨质谱测定,内标法定量。结果表明,该方法对于酱油中4种氯丙醇的定量限为0.5~10 μg/kg。在3个浓度水平下的加标回收率为78%~103%;相对标准偏差均不大于8.8%。该方法快速、简便、准确、灵敏,可作为酱油中4种氯丙醇的有效检测方法。

关键词: 分散固相萃取, 气相色谱-高分辨质谱, 氯丙醇, 酱油

Abstract: A method for the rapid screening of 1,3-dichloro-2-propanol, 2,3-dichloro-1-propanol,3-monochloropropane-1,2-diol, and 2-monochloropropane-1,3-diol in soy sauce was developed based on dispersive solid phase extraction-gas chromatography-high resolution mass spectrometry (GC-HRMS). The samples were extracted by ethyl acetate, cleaned up using N-propylethylenediamine and detected by GC-HRMS. The chloropropanols were quantified by the internal standard method. The results demonstrated that the limits of quantitation of the four chloropropanols were in the range of 0.5-10 μg/kg. The recoveries of the four chloropropanols in soy sauce spiked with three levels varied from 78% to 103%, and the relative standard deviations were no more than 8.8%. The proposed method is simple, accurate, sensitive and suitable for the rapid screening of the four chloropropanols in soy sauce.

Key words: dispersive solid phase extraction, gas chromatography-high resolution mass spectrometry (GC-HRMS), chloropropanol, soy sauce

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