气相色谱-质谱联用法测定瓶装水中邻苯二甲酸酯的含量
目的 建立市售瓶装水中邻苯二甲酸酯类化合物的 GC-MS/MS 分析方法, 研究包装材料种类、保存条件对瓶装水中邻苯二甲酸酯类化合物浓度的影响。方法 样品经固相萃取净化(SPE)、二氯甲烷洗脱, 真空浓缩后, 采用 GC-MS/MS 对 16 种邻苯二甲酸酯类化合物进行检测, 同位素内标定量。结果 16 种化合物在20~500 ng/mL 浓度范围内, 线性关系良好, 相关系数 R2大于 0.996。在 200、50 ng/mL 两个加标水平下, 方法回收率为 71%~109%, RSD 小于 5%。方法最低检测限在 7.25~11.93 ng/L 范围内, 市售的 29 个品牌的瓶装水中均检出 DEHP(≥20 ng/L), 25 个 PET 瓶装水中均检出 DEHP、DIBP 和 DBP, 在高温保存条件下, 瓶装水中的邻苯二甲酸酯类化合物含量会显著提高。 结论 该方法适用于瓶装水中邻苯二甲酸酯类化合物的测定, 本研究为开展瓶装水中邻苯二甲酸酯类化合物的风险评估提供参考。
Objective To establish a method for determination of phthalates esters in bottled waters by gas chromatography coupled with tandem mass spectrometry (GC-MS/MS), and study the effect of the kinds of packaging materials and storage conditions on the concentration of phthalate esters in bottled water. Methods The bottled waters were cleaned up by SPE column, eluted with dichloromethane, concentrated by vaccum rotation evaporimeter, and analyzed by GC-MS/MS. The isotope internal standards were applied to the analysis and quantitation of phthalate esters. Results The method showed a good linearity over the range of 20~500 ng/mL for 16 compounds of phthalate esters with R2≥0.996. The detection limit was 7.25~11.93 ng/L. The recoveries were 74%~106% at the spiked level of 200 ng/mL and 50 ng/mL with relative standard deviation lower than 5%. Phthalate esters were detected in 29 brands of bottled waters sold in Shanghai, and the concentration of DEHP was higher than 20 ng/L. DEHP, DIBP and DBP were detected in 25 brands of bottled waters with the packing material of PET. When stored at high temperature, the concentration of phthalate esters in bottled water raised sharply. Conclusion This method is suitable for the analysis of phthalate esters, and it provides a reference for the risk evaluation of phthalate esters in bottled water.
标题：气相色谱-质谱联用法测定瓶装水中邻苯二甲酸酯的含量
英文标题：Determination of phthalates esters in bottled waters by GC-MS/MS
作者：
汪国权 上海疾病预防控制中心
邱歆磊 上海疾病预防控制中心
冯超 上海疾病预防控制中心
中文关键词:市售瓶装水,邻苯二甲酸酯类化合物,气相色谱-质谱联用法,
英文关键词:bottled water,phthalate esters,gas chromatography-tandem mass spectrometry,
发表日期：2013-05-22
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