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

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0.5~10μg/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。

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

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.