摘要
目的建立植物油中氯丙醇脂肪酸酯(包括3-MCPD酯、2-MCPD酯)的同位素稀释气相色谱-质谱(GCMS)检测方法。方法样品经甲醇钠-甲醇溶液进行酯键断裂反应后,用硅藻土小柱进行固相支持液液萃取净化,净化液经七氟丁酰基咪唑衍生后用GC-MS检测,以氘代同位素标准品为内标,内标法定量。结果 3-MCPD酯、2-MCPD酯的浓度为25μg/L^1 000μg/L时,线性关系良好,相关系数(r)均>0.999 5。3-MCPD酯、2-MCPD酯的检出限均为100μg/kg。以空白食用植物油在250μg/kg、500μg/kg、1 000μg/kg水平的加标回收率为93.2%~110.8%,相对标准偏差(RSD)为2.3%~4.8%。结论该方法简便、准确、可靠,适用于食用植物油中氯丙醇脂肪酸酯含量的测定。通过对93份食用植物油样品的测定,初步得到杭州市食用植物油中氯丙醇酯的污染特征;通过植物油摄入氯丙醇酯的健康风险需引起关注。
Objective To establish a method for the determination of fatty acid esters of chloropropanols（ including 3- MCPD esters,2- MCPD esters） in edible vegetable oil by isotope dilution- gas chromatography- mass spectrometry（ GC- MS）.Methods The oil sample was conducted for ester- bond cleavage reaction with sodium methylate- methanol and purified by matrix solid- supported liquid- liquid extraction. After derivation with heptafluoro butyrylimidazole（ HFBI）,the target analytes were determined by GC- MS,with deuterium isotopes standard as the internal standard and internal standard for quantification.Results Good linearity was obtained when the concentrations of 3- MCPD esters,2- MCPD esters were within 25 μg / L-1 000 μg / L,with coefficient correlations（ r） 0. 999 5. The limits of detection（ LODs） for 3- MCPD esters,2- MCPD esters were 100 μg / kg. The average recoveries of chloropropanols esters spiked at 250 μg / kg,500 μg / kg and 1 000 μg / kg in edible vegetable oil were typically within 93. 2%- 110. 8%,with relative standard deviations（ RSDs） within 2. 3%- 4. 8%. Conclusion This method is simple,accurate and reliable,which is suitable for the determination of fatty acid esters of chloropropanols in edible vegetable oil. The pollution characteristics in edible vegetable oil in Hangzhou was preliminarily acquired by the determination of 93 samples. Results show that the health risks by chloropropanols esters intake from edible vegetable oil should be concerned.
出处
《中国卫生检验杂志》
CAS
2016年第21期3093-3097,共5页
Chinese Journal of Health Laboratory Technology
关键词
食用植物油
脂肪酸氯丙醇酯
气相色谱-质谱
Edible vegetable oil
Fatty acid esters of chloropropanols
Gas chromatography-mass spectrometry
