盐析辅助液液萃取结合气相色谱-质谱法测定酱油中4种氯丙醇

Determination of 4 kinds of chloropropanols in soy sauce by salting-out assisted liquid-liquid extraction combined with gas chromatography-mass spectrometry

中文关键词:  酱油  氯丙醇  盐析辅助液液萃取  气相色谱-质谱法

英文关键词:soy sauce  chloropropanols  salting-out assisted liquid-liquid extraction  gas chromatography-mass spectrometry

中文摘要:

      目的 建立盐析辅助液液萃取结合气相色谱-质谱法测定酱油中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-丙二醇的分析方法。方法 以D5-3-氯-1,2-丙二醇为内标物, 酱油样品经乙腈提取, 氯化钠盐析分层, 七氟丁酰基咪唑衍生, HP-5MS毛细管柱(30 m×0.25 mm, 0.25 μm)分离, 采用气相色谱-质谱法的选择离子监测模式进行测定。实验考察了盐析助剂、萃取溶剂对4种氯丙醇萃取效率的影响。结果 最优实验条件下, 4种氯丙醇在0.006~0.120 mg/kg范围内线性关系良好, 且相关系数都大于0.999, 检出限为0.002 mg/kg, 定量限为0.006 mg/kg。在0.02、0.05、0.10 mg/kg的加标水平下, 4种氯丙醇的加标回收率为70.2%~103.5%, 相对标准偏差为1.6%~5.5%。结论 本方法快速、简便、节省溶剂, 适用于酱油中氯丙醇的快速定性、定量分析。

英文摘要:

      Objective To establish a method for the determination of 1,3-dichloro-2-propanol, 2,3-dichloro-1-propanol, 3-chloro-1,2-propanediol and 2-chloro-1,3-propanediol in soy sauce based on salting-out assisted liquid-liquid extraction coupled with gas chromatography-mass spectrometry. Methods Using 3-chloro-1,2-propanediol-d5 as deuterated internal standard, the soy sauce sample was extracted with acetonitrile, salted out by sodium chloride, derived using 1-(heptafluorobutyryl)imidazole, separated by HP-5MS capillary column (30 m×0.25 mm, 0.25 μm) and determined by gas chromatography-mass spectrometry in selected ion monitoring mode. The effects of salting-out aid and extraction solvent on extraction efficiency of the 4 kinds of chloropropanols were investigated. Results Under the optimal experimental conditions, the 4 kinds of chloropropanols showed good linearity in the range of 0.006–0.120 mg/kg, and the correlation coefficients were all above 0.999, and the limits of detection of the 4 kinds of chloropropanols were 0.002 mg/kg, and the limits of quantitation were 0.006 mg/kg. The recoveries of the 4 kinds of chloropropanols were in the range of 70.2%–103.5%, and the relative standard deviations were in the range of 1.6%–5.5% at the spiked levels of 0.02, 0.05 and 0.10 mg/kg. Conclusion This method can provide a good specificity for the rapid qualitative and quantitative analysis of chloropropanols in soy sauce with the advantage of rapid, simple and solvent saving.