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目的建立膳食样品中3-氯-1-2-丙二醇(3-MCPD)酯和2-氯-1,3-丙二醇(2-MCPD)酯的固相支持液液萃取-气相色谱-质谱(SLE-GC-MS)检测方法。方法膳食样品经正己烷超声提取,用甲醇钠/甲醇水解后,以硅藻土作为吸附剂进行固相支持液液萃取净化,经七氟丁酰咪唑衍生后,进行GC-MS测定,采用氘代同位素标准进行内标法定量。结果 3-MCPD酯和2-MCPD酯在不同膳食样品中的检出限分别为0.002~0.005 mg/kg和0.002~0.006 mg/kg,膳食样品中3-MCPD酯和2-MCPD酯在0.05 mg/kg和0.1 mg/kg水平的加标回收率分别为65.9%~104.2%和75.4%~118.0%,相对标准偏差分别为2.2%~14.2%和0.8%~13.9%。结论该方法简便、准确、可靠,适用于膳食样品中3-MCPD酯和2-MCPD酯的检测。
OBJECTIVE To establish a solid phase liquid-liquid-liquid chromatography-gas chromatography-mass spectrometry (SLE) system for the determination of 3-MCPD and 2-MCPD esters in dietary samples. -GC-MS) detection method. Methods The dietary samples were extracted by n-hexane, hydrolyzed by sodium methoxide / methanol, and purified by liquid-liquid extraction with solid-phase support using diatomaceous earth as adsorbent. After derivatization with heptafluorobutyryl imidazole, GC- A isotope standard for internal standard quantification. Results The detection limits of 3-MCPD ester and 2-MCPD ester in different dietary samples were 0.002-0.005 mg / kg and 0.002-0.006 mg / kg respectively. The concentrations of 3-MCPD ester and 2-MCPD ester in dietary samples were 0.05 mg The recoveries of spiked samples ranged from 65.9% to 104.2% and from 75.4% to 118.0% at the levels of 0.1 mg / kg and kg, respectively. The relative standard deviations were 2.2% -14.2% and 0.8% -13.9%, respectively. Conclusion The method is simple, accurate and reliable and is suitable for the determination of 3-MCPD ester and 2-MCPD ester in dietary samples.