气相色谱-三重四极杆质谱法测定液体乳及乳粉中的17种邻苯二甲酸酯类增塑剂

Determination of 17 Phthalic Acid Esters in Milk and Milk Power by Gas Chromatography-Tandem Mass spectrometry

中文关键词:  GC-MS/MS  乳与乳制品  邻苯二甲酸酯

英文关键词:GC-MS/MS  milk and milk power  phthalic acid esters

中文摘要:

      建立了液体乳及乳粉中17种邻苯二甲酸酯类增塑剂同时测定的气相色谱-三重四极杆质谱( GC-MS/MS) 方法。样品经乙腈超声提取,凝胶渗透色谱(GPC)净化后用GC-MS/MS分析,外标法定量。该方法线性关系良好,相关系数为0.9956~0.9999；方法的检出限(S/N=3)为3 μg/kg～60 μg/kg；定量限(S/N=10)为10 μg/kg～200 μg/kg；在50、200、500 μg/kg添加水平下的平均回收率为 78.2%～115.4 %,相对标准偏差为 2.65 %～9.95 %。采用该方法对36个市售液体乳及乳粉进行测定,其中22个样品检出多种邻苯二甲酸酯类增塑剂。

英文摘要:

      A gas chromatography-tandem spectrometry method was established for the simultaneous determination of 17 phthalics acid esters (PAEs) in milk and milk power. The samples were extracted by acetonitrile in an ultrasonator, purified by gel permeation chromatography (GPC), and determined by GC-MS/MS using external stangard method. The results exhibited good linear relationship with the correlation coefficients of 0.9956-0.9999; the limits of detection (LODs, S/N=3) for the 17 PAEs were in the range of 3 μg/kg～60 μg/kg, and the limits of quantitation (LOQs, S/N=10) were in the range of 10 μg/kg～200 μg/kg; the average recoveries of 17 PAEs at three spiked levels of 50, 200, 500 μg/kg were between 78.2% and 115.4%, with relative standard deviations of 2.65%-9.95%. The proposed method was applied in the determination of PAEs in 36 commercially available milk and milk power products, and 22 of which were detected containing phthalate plasticizers.