气相色谱-质谱法测定婴幼儿配方乳粉及原料中15种邻苯二甲酸酯

Determination of 15 phthalic acid esters in infant formula milk powder and raw material by gas chromatography-mass spectrometry

目的建立婴幼儿配方乳粉及原料中15种邻苯二甲酸酯的气相色谱-质谱检测方法。方法样品经乙腈提取后,用GC-MS检测。采用外标法进行定量分析。结果 15种邻苯二甲酸酯的线性范围除了邻苯二甲酸二异壬酯为0.01～1 mg/L,其余均为0.001～1 mg/L,相关系数大于0.99。方法检出限(S/N=3)为0.006～0.2 mg/kg,定量限(S/N=10)为0.02～0.7 mg/kg。在奶粉基质中3个加标水平下邻苯二甲酸酯的平均回收率在88.6%～117.2%,相对标准偏差为1.0%～9.3%。结论本方法操作简单、精确、快速、廉价、稳定,适用于奶粉中邻苯二甲酸酯类化合物的检测分析。

Objective To establish a method for determination of phthalic acid esters in infant formula milk powder and raw materials by gas chromatography-mass spectrometry(GC-MS).Methods Samples were extracted with acetonitrile,and then detected by GC-MS.The external standard method was conducted for the quantitative analysis.Results The linear range of 15 phthalic acid esters were 0.001~1 mg/L,except that the linear range of phthalate isononyl ester was 0.01~1 mg/L with R>0.99.LOD(S/N=3) and LOQ(S/N=10) were 0.006~0.2 mg/kg and 0.02~0.7 mg/kg,respectively.The recoveries were 88.6%~117.2% at three spiked level with relative standard deviation of 1.0%~9.3%.Conclusion This method is simple,accurate,fast,cheap and stable,and it is suitable for the detection of phthalic acid esters in milk powder.