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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 the determination of 15 kinds of phthalates in infant formula milk powder and raw materials by gas chromatography-mass spectrometry. Methods Samples were extracted with acetonitrile and detected by GC-MS. External standard method for quantitative analysis. Results The linear range of 15 kinds of phthalates was 0.01-1 mg / L for diisononyl phthalate and 0.001-1 mg / L for the rest. The correlation coefficient was greater than 0.99. The limit of detection (S / N = 3) was 0.006-0.2 mg / kg and the limit of quantitation (S / N = 10) was 0.02-0.7 mg / kg. The average recoveries of phthalates at three spiked levels in the milk powder matrix ranged from 88.6% to 117.2% with relative standard deviations of 1.0% to 9.3%. Conclusion The method is simple, accurate, rapid, inexpensive and stable and is suitable for the detection and analysis of phthalates in milk powder.