固相萃取-衍生化-气相色谱-质谱法测定富脂调味品中3-氯-1,2-丙二醇  

Determination of 3-monochloropropane-1,2-diol in grease food by solid phase extraction-derivatization-gas chromatography-mass spectrometry

作　　者：向晓玲[1] 王立媛[2] 沈向红[2] 李春松 沈建福[1] 吴平谷[2] 

机构地区：[1]浙江大学生物系统工程与食品科学学院,杭州310058 [2]浙江省疾病预防控制中心 [3]金华市食品药品检验检测研究院

出　　处：《卫生研究》2017年第5期777-782,共6页Journal of Hygiene Research

基　　金：浙江省分析测试科技计划项目(No.2016C37013)

摘　　要：目的建立固相萃取-衍生化-气相色谱-质谱法测定富脂调味品中的3-氯-1,2-丙二醇(3-MCPD)的方法。方法以豆瓣酱等为代表的富脂调味品采用超声提取,碱性硅藻土固相萃取柱净化、苯硼酸衍生后采用气相色谱质谱法(GC-MS)测定3-MCPD。结果 3-MCPD的线性范围为1~100 ng/mL,相关系数为0.9993,3-MCPD在酱油、黄豆酱、辣椒油3种基质中的检出限分别为0.6、0.5和7.0μg/kg,定量限分别为1.9、1.6和18.8μg/kg。在样品中添加2.5~1000μg/kg 3-MCPD,平均回收率为78.3%~106.7%,相对标准偏差为1.9%~11.6%(n=6)。结论该方法净化效果好,灵敏度、准确度均满足检测要求,可作为富脂调味品中3-MCPD含量检测的确证方法。Objective To establish the method of determination of 3-monochloropropane-1,2-diol（ 3-MCPD） in grease food by gas chromatography-mass spectrometry（ GC-MS）. Methods 3-MCPD in grease food represented by bean paste was extracted by ultrasound,purified by alkaline earth solid phase extraction column,derivatived using phenylboronic acid（ PBA） and detected by GC-MS. Results The linearity of 3-MCPD ranged from 1-100 ng/mL,with correlation coefficient at 0. 9993.The limits of quantitation（ LOQ） in soy sauce,bean paste,pepper oil were 0. 6,0. 5 and7. 0 μg/kg and limits of detection（ LOD） were 1. 9,1. 6 and 18. 8 μg/kg,respectively.Average recovery rate and relative standard deviation was 78. 3%-106. 7% and 1. 9%-11. 6%（ n = 6）, when 3-MCPD was added in grease food at 2. 5-1000 μg/kg.Conclusion The method has good purification effect and the detection sensitivity and accuracy,and can be used for the determination of 3-MCPD in grease food.

关 键 词：固相萃取 苯硼酸 衍生化 3-氯-1 2-丙二醇 

分 类 号：TS207.5[轻工技术与工程—食品科学] TS264.2[轻工技术与工程—食品科学与工程]