| 摘要: |
| 建立了测定食品接触材料中6种邻苯二甲酸酯的含量的高效液相色谱-串联质谱法（HPLC-MS/MS）。实验以Agilent ZORBAX SB-C18色谱柱为分析柱，以甲醇-0.1%的甲酸水为流动相，采用梯度模式洗脱。质谱离子源的工作模式为正离子电离模式（ESI+），流速为0.35 mL/min，采用多反应监测离子模式（MRM）进行检测定量。实验样品前处理采用了加速溶剂萃取法，明显提高了食品接触材料中邻苯二甲酸酯的提取效率。结果表明：6种邻苯二甲酸酯在其线性范围内线性关系良好（R2＞0.999），DPRP和BBP的定量限为1.0 ng/mL，DCHP，DNHP，DHP，DBEP的定量限为0.2 ng/mL，DPRP和BBP的检测限为0.2 ng/mL，DCHP，DNHP，DHP，DBEP的检测限为0.05 ng/mL。该方法的加标回收率为89.2%~107.5%，相对标准偏差均小于5.0%。实验表明，所建立的方法简单、灵敏度高，适用于食品接触材料中的6种邻苯二甲酸酯类增塑剂的分析检测。 |
| 关键词: 邻苯二甲酸酯 高效液相色谱-串联质谱法 食品接触材料 |
| DOI： |
| 分类号:TB487; TS206 |
| 基金项目: |
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| Determination of 6 Phthalates in Food Contact Materials by HPLC-MS/MS |
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DING Li1, XIAO Jia-yong1, LONG Yan-jiao2, FU Shan-liang1, WANG Xiao-bing3, WANG Li-bing1
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1.Technology Center of Hunan Entry-Exit Inspection and Quarantine Bureau, Hunan Key Laboratory of Food Safety Science & Technology, Changsha 410004, China;2.Guangdong Entry-Exit Inspection and Quarantine Bureau, Guangzhou 510623, China;3.China Petroleum and Chemical Industry Federation, Beijing 100029, China
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| Abstract: |
| A high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was established and validated for simultaneous determination of 6 phthalates in food contact materials. The analytes were separated by an Agilent ZORBAX SB-C18 column with a mobile phase of methanol-water in gradient elution mode at the flow rate of 0.35 mL/min, in which the water phase was added 0.1% formic acid, the mass spectrometry worked in positive ion mode and MRM was adopted for quantification of the analytes. Besides, samples were extracted with accelerated solvent extraction, which significantly increased extraction efficiency of phthalates from food contact materials. The results showed a good linearity for 6 phthalates under the optimal conditions. The correlation coefficients were all more than 0.999; the limits of quantification of the method is 1.0 ng/mL for DPRP, BBP and 0.2 ng/mL for DCHP, DNHP, DHP, and DBEP; detection limit is 0.2 ng/mL for DPRP, BBP and 0.05 ng/mL for DCHP, DNHP, DHP, and DBEP; average recoveries of the 6 analytes at three spiked level ranged from 89.2% to 107.5%, with RSD less than 5.0%. The method is sensitive and simple, and is suitable for determination of the 6 phthalates in food contact materials. |
| Key words: phthalates high performance liquid chromatography-tandem mass spectrometry food contact materials |
