摘要
文章通过冷冻、低温离心和固相萃取等前处理过程的优化,消除含油调味样品中的干扰物,建立气质联用同位素内标法测定样品中3-氯-1,2-丙二醇。将该方法用于检测实际富含油脂调味样品中的3-氯-1,2-丙二醇,结果令人满意。其方法检出限为0.031mg/kg,线性相关系数为0.9992,加标回收率为80.0%~89.0%,精密度为3.76%~4.05%。
Optimize the pre-processing by freezing,low-temperature centrifugation and solid-phase extraction,eliminate the interferences in the oily condiments,establish isotopic internal standard method for the determination of 3-chlorine-1,2-propylene glycol by GC-MS.This method is applied for the actual samples' analysis with satisfactory results.The detection limit is 0.031 mg/kg,the linearly dependent coefficient is 0.9992,the recovery rate is 80.0%~89.0%,the precision is 3.76%~4.05%.
引文
[1]江新业.酸水解植物蛋白调味液中氯丙醇的危害与控制[J].中国食品添加剂,2013(S1):164-171.
[2]GB 2762-2012,食品中污染物限量[S].
[3]吴少明,傅武胜,傅海庆,等.多同位素内标气相色谱-质谱法测定食品中4种氯丙醇含量[J].食品科学,2013,34(18):131-136.
[4]吴小琼,陈中文,管健,等.固相萃取-同位素内标GC-MS法测定酱油中的4种氯丙醇[J].中国卫生检验杂志,2014,24(10):1422-1424.
[5]刘伟,李兵,赵榕,等.固相萃取-气相色谱质谱联用法测定酱油中3种氯丙醇类污染物[J].中国食品卫生杂志,2011,23(5):425-428.
[6]车巨龙,樊晓红.气质联用测定酱油中氯丙二醇研究[J].山西化工,2015,35(1):47-49.
[7]廖华勇,鲍伦军.气相色谱同时检测调味品中三种氯丙醇的方法研究[J].中国卫生检验杂志,2001,11(6):647-650.
[8]张明霞,陈雪桥,周建科.气相色谱法检测汤料中氯丙醇类化合物[J].理化检验(化学分册),2007(11):953-955.
[9]晏雨微.3-氯-1,2-丙二醇的HPLC-FLD法测定及前处理材料的合成与评价[D].武汉:武汉轻工大学,2014.