气相色谱-质谱法检测乳与乳制品中20种邻苯二甲酸酯.pdfVIP

21 2013, Vol.36 No.6 乳业科学与技术 ※分析检测 气相色谱-质谱法检测乳与乳制品中20种 邻苯二甲酸酯 * 许卫萍，胡 雪，李翠枝 ，邵建波，高玉杰 ( 内蒙古伊利实业集团股份有限公司，内蒙古 呼和浩特 0 100 10) 摘  要：建立了乳与乳制品中20种邻苯二甲酸酯气相色谱-质谱联用仪分析方法。样品用正己烷提取后，采用DB- 5MS(30m ×0.25mm ，0.25μm)石英毛细管柱分离，在进样口温度280 ℃，传输线温度280 ℃，离子源温度230 ℃条件 下20种邻苯二甲酸酯完全分离。该方法各组分的相关系数均大于0.9990 ，线性范围0～10μg/mL ，样品加标回收率 为80%～109% 。邻苯二甲酸二异壬酯、邻苯二甲酸二异癸酯化合物检出限分别为1.0 、0.5mg/kg ，其他化合物均为 0.05mg/kg 。该方法具有简单易行，快速准确，灵敏度高等优点。 关键词：气相色谱-质谱法(GC-MS) ；邻苯二甲酸酯；乳与乳制品 Determination of 20 Phthatic Acid Esters in Milk and Dairy Products by GC-MS * XU Wei-ping, HU Xue, LI Cui-zhi , SHAO Jian-bo, GAO Yu-j ie (Inner Mongolia Yili Industrial Group Co. Ltd., Hohhot 0 100 10, China) Abstract: A method was developed for the determination of 20 phthatic acid esters in milk and dairy products by gas chromatography-mass spectrometry (GC-MS). Samples were extracted with n-hexane and separated on a DB-5MS capillary column (30 m ×0.25 mm, 0.25 μm). The inj ector temperature was 280 ℃,the interface temperature was 280 ℃, and the ion source temperature was 230 ℃. Under optimized conditions, the linear range was 0-10 μg/mL with a correlation coefficient greater than 0.9990. The average spike recovery rates were in the range of 80%-109%. The detection limits were respectively 1.0 and 0.5 mg/kg for DINP and DIDP and 0.05 mg/kg for 18 others. This method proved to be simple, rapid, sensitive, specific and accurate. Key words: gas chromatography-mass spectrometry (GC-MS); phthatic acid esters; milk and dairy products 中图分类号：TS252.7                    文献标志码：A 文章编号：1671-5187(2013)06-0021-03 邻苯二甲酸酯(phthalic acid