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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 an isotope dilution gas chromatography-mass spectrometry (GCMS) method for the determination of chloropropanol fatty acid esters (including 3-MCPD esters and 2-MCPD esters) in vegetable oils. Methods After the ester bond cleavage reaction was carried out in sodium methylate-methanol solution, the sample was purified by liquid-liquid extraction with solid-phase support on a small column of diatomaceous earth. The purified liquid was determined by GC-MS after derivatization with heptafluorobutyrylimidazole. The deuterated isotope Standard internal standard, internal standard method. Results When the concentration of 3-MCPD ester and 2-MCPD ester was 25μg / L to 1 000μg / L, the correlation coefficient was good (r)> 0.999. The detection limits of 5.3-MCPD ester and 2-MCPD ester Both were 100 μg / kg. The spiked recoveries of blank edible vegetable oil at the levels of 250μg / kg, 500μg / kg and 1000μg / kg were 93.2% ~ 110.8% with relative standard deviations (RSDs) of 2.3% -4.8%. Conclusion The method is simple, accurate and reliable and is suitable for the determination of chloropropanol fatty acid esters in edible vegetable oils. Through the determination of 93 samples of edible vegetable oil, the pollution characteristics of chloropropanol ester in edible vegetable oil in Hangzhou were preliminarily obtained. The health risks of chloropropanol ester intake by vegetable oil should be concerned.