SPE-GC-MS法测定固态调味品中3-氯-1,2-丙二醇

Determination of 3-chloro-1,2-propanediol in solid condiments by SPE-GC-MS

目的:建立了固相萃取-气相色谱-质谱法测定固态调味品中的3-氯-1,2-丙二醇的检测方法。方法:样品经乙醚提取,经SPE柱净化,用七氟丁酰基咪唑作为衍生化试剂,采用非极性毛细管色谱柱DB-5MS分离,GC-MS选择离子监测模式(SIM)测定,同位素内标定量。结果:3-氯-1,2-丙二醇线性范围为0.001~1.0 mg/kg,相关系数r为0.9998,相对标准偏差RSD为0.4~9.2%,检测下限为0.001 mg/kg,4种不同类型样品的加标回收率为81.0~104%。对鸡精、味精、鸡粉、香辛料粉、猪骨高汤粉、方便面调味料、其他调味料等7类,共30批固态调味品,进行3-氯-1,2-丙二醇含量的检测,发现复合香辛料中没有检出3-氯-1,2-丙二醇,而其他调味料中均有3-氯-1,2-丙二醇检出,含量在3.92~856 μg/kg。结论:该方法减少了有机溶剂的消耗,节省了前处理的时间,且灵敏度高,结果准确,适合批量测试,能满足日常固态调味品中3-氯-1,2-丙二醇的检测。

Objective :To establish a solid phase extraction-gas chromatography-mass spectrometry method for the determination of 3-chloro-1,2-propanediol in solid condiments. Methods:The sample was extracted with ether,and purified by SPE column;heptafluorobutyryl imidazole was used as the derivatization reagent,and samples were then separated by non-polar capillary column DB-5MS and determined by GC-MS selective ion detection mode(SIM),using isotope internal standard quantification method. Results:The linear range of 3-chloro-1,2-propanediol was 0.001 ~ 1.0 mg/kg,correlation coefficient r was 0.9998,relative standard deviation RSD was 0.4 ~ 9.2%,and detection limit was 0.001 mg/kg. The recovery rate of standard addition was 81.0 ~ 104%. A total of 30 batches of solid condiments in 7 categories were tested,including chicken essence,monosodium glutamate,chicken powder,spice powder,pork bone stock powder,instant noodle seasoning,and other seasonings. No 3-chloro-1,2-propanediol was detected in compound spices,while it was detected in other seasonings with the content of 3.92 ~ 896 μg/kg. Conclusion:This method reduced the amount of organic solvents and pretreatment time. It was highly sensitive and accurate. It is suitable for large amount of sample testing and can meet daily needs of detecting 3-chloro-1,2-propanediol in solid condiments.