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〔目的〕建立了GC -ECD同时分析调味品中三种氯丙醇的方法。〔方法〕采用柱层析方法 ,用乙醚及正已烷和乙醚 (1+1,v/v)的混合液对样品进行提取与净化 ,经七氟丁酰口米唑衍生 ,最后通过GC -ECD测定调味品中氯丙醇的含量。〔结果〕通过对实验条件的优化 ,本法可以同时测定调味品中的 1,3_二氯_2_丙醇、2 ,3_二氯_1_丙醇和 3-氯_1,2_丙二醇 ,检出限为 0 .0 1mg/kg。当氯丙醇的添加范围在 0 .0 1～ 0 .5mg/kg时 ,1,3_二氯_2_丙醇 (1,3-DCP)的回收率可达 89.5 %～ 97.5 % ;2 ,3_二氯_1_丙醇 (2 ,3-DCP)的回收率可达 93.8%～ 10 0 .8% ;3_氯_1,2_丙二醇 (3_MCPD)的回收率可达 90 .4%～ 10 2 .1%。〔结论〕该方法准确、快速、灵敏度高。
[Objective] To establish a method for simultaneous determination of three chloropropanols in condiments by GC-ECD. [Method] The sample was extracted and purified by column chromatography with diethyl ether and a mixture of n - hexane and diethyl ether (1 + 1, v / v), derivatized with heptafluorobutyloxazole and finally detected by GC - ECD determination of condiment chloropropanol content. [Results] Through the optimization of the experimental conditions, this method can simultaneously determine the condiment 1,3_ dichloro_2_ propanol, 2,3_ dichloro_1_ propanol and 3-chloro _1,2_ Propylene glycol, detection limit of 0 1mg / kg. The recovery of 1,3-dichloro-2-propanol (1,3-DCP) reached 89.5% -97.5% when the addition of chloropropanol was in the range of 0.01 ~ 0.5mg / kg. , 3_ dichloro_1_ propanol (2,3-DCP) recovery of up to 93.8% ~ 108.8%; 3_ chlorine _1,2_ propylene glycol (3_MCPD) recovery of up to 90%. 4% ~ 10 2 .1%. Conclusion The method is accurate, rapid and sensitive.