同位素稀释-气相色谱-质谱法测定白酒中23种邻苯二甲酸酯类化合物

GC-MS Determination of 23 Phthalate Esters in Liquor by Isotope Dilution

提出了同位素稀释-气相色谱-质谱法测定白酒中23种邻苯二甲酸酯类化合物含量的方法。样品用正己烷-乙酸乙酯(1+1)混合液提取后,经DB-5MS毛细管色谱柱分离,采用电子轰击离子源选择离子反应监测模式进行质谱测定,同位素内标法进行定量分析。23种邻苯二甲酸酯类化合物的线性范围在0.2~3.0mg·L-1之间,测定下限(10S/N)在0.05~0.1mg·kg-1之间。加标回收率在73.2%~122%之间,相对标准偏差(n=6)在0.49%~11%之间。

Isotope dilution gas chromatography-mass spectrometry(GC-MS) was applied for the determination of 23 phthalate esters in liquor.The sample was extracted with a mixture(1+1)of n-hexane and ethyl acetate,and separated by DB-5MS capillary chromatographic column.EI and SIM were adopted in MS detection.Isotope internal standard method was used for quantization.Linearity ranges of the 23 phthalate esters were between 0.2-3.0mg·L-1,and the quantization limits(10S/N)were between 0.05-0.1mg·kg-1.Values of recovery and RSD′s(n=6)were in the range of 73.2%-122% and 0.49%-11% respectively.