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

中文关键词:  气相色谱-质谱  邻苯二甲酸酯  婴幼儿配方乳粉

英文关键词:gas chromatography-mass spectrometry  phthalic acid esters  infant formula milk powder

中文摘要:

      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。

英文摘要:

       Objective To establish a method for the 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.