摘要
目的建立食用植物油中3-氯丙醇酯的GC-MS测定方法,并对83份深圳市售食用植物油中3-氯丙醇酯的含量进行调查。方法称取0.1 g样品,以1 ml甲醇钠甲醇溶液（0.25 mol/L）将脂肪中的3-氯丙醇酯（3-MCPD酯）水解成3-氯丙醇（3-MCPD）,用硅藻土小柱净化后,经七氟丁酰基咪唑衍生后,用选择离子监测的气相色谱-质谱联用法测定,采用内标法定量。结果 3-MCPD酯在250~5 000μg/kg范围内线性良好（r〉0.999）,3个浓度水平下加标回收率为78.5%~99.8%,相对标准偏差为2.5%~6.0%。83份食用植物油样品中,检出率60%,3-氯丙醇酯含量为0~1.72 mg/kg。结论方法准确度高、灵敏度高,适合食用植物油中3-氯丙醇酯的检测。
Objective To establish a method for determination of 3-chloro-1,2-propanediol（ 3-MCPD） esters in vegetable oils by GC-MS and investigate 3-MCPD esters residues in 83 vegetable oils from supermarkets. Methods 3-MCPD esters were extracted from 0. 1 g of the samples and hydrolyzed into 3-MCPD with 1. 0 m L of sodium methylate solution（ 0. 25 mol / L,in methanol）. Following purification using diatomaceous earth columns and derivation with heptafluorobutyrylimidazole（ HFBI）,analytes were determined by GC-MS under SIM mode and quantified by internal standard method. Results The linearity was good over the range of 25-5000 μg / kg（ r 0. 999）; recoveries at three concentration levels were 78. 5%-99. 8%,the relative standard derivations were2. 5%-6. 0%. Among the 83 vegetable oil samples,3-MCPD esters were detected from 60% and the contents were within the range of 0-1. 72 mg / kg. Conclusion The method has high sensitivity and accuracy and is suitable for determination of 3-chloro-1,2-propanediol esters in vegetable oils.
出处
《预防医学情报杂志》
CAS
2016年第9期912-915,共4页
Journal of Preventive Medicine Information
基金
深圳市科技创新委员会知识创新计划基础研究项目"深圳市居民膳食中新型污染物氯丙醇酯的暴露状况研究"(No:JCYJ20140410170519145)
