保和丸中外源性邻苯二甲酸酯类的检测-中国药事.pdf

中国药事 2017 年 4 月 第 31 卷 第 4 期 441 保和丸中外源性邻苯二甲酸酯类的检测 姚羽，张琳，王文艳，马敏 （山西省食品药品检验所，太原 030001） 摘要 目的：为考察聚氯乙烯固体药用硬片中邻苯二甲酸酯类（PAEs）向保和丸中迁移情况，建立了检 测方法。方法：采用 Elite-5（30 m×0.32 mm，0.25 μm）毛细管色谱柱，氢火焰离子化检测器（FID）， 进样温度为 250 ℃，检测器温度为 300 ℃，载气为氮气，程序升温，不分流进样，进样量为 1 μL。并结 合气相色谱 - 质谱法（GC-MS）对样品中的 PAEs 进行定性确认。结果：6 种 PAEs 在各自的浓度范围内 r n 呈良好线性关系， 为 0.9994 ~ 0.9999，平均加样回收率为 96.8% ~ 100.4% （ =9，RSD 均小于 3.0% ）。 3 批样品的包材和药品中均有 PAEs 检出。结论：该方法分离效果好、操作简便、快速、灵敏度高、精密 度好，适用于保和丸中 6 种 PAEs 的同时测定。样品的加速试验表明，聚氯乙烯固体药用硬片中的 PAEs 存在向药品迁移的现象。 关键词： 药包材质量；酞酸酯；聚氯乙烯材料；增塑剂；GC；保和丸；GC-MS；药品包装安全性 中图分类号：R917 文献标识码：A 文章编号： 1002-7777(2017)04-0441-06 doi:10.16153/j.1002-7777.2017.04.016 Detection of Exogenous Phthalate Esters in Baohe Pills Yao Yu, Zhang Lin, Wang Wenyan, Ma Min (Shanxi Institute for Food and Drug Control, Taiyuan 030001, China) Abstract Objective: To determine the migration of phthalate esters (PAEs) in polyvinyl chloride (PVC) sheet with solid pharmaceutical packaging to Baohe pills, so as to establish a detection method. Methods: The PAEs solvents were separated on Elite-5 capillary column (30 m × 0.32 mm, 0.25 μm). FID was used as detector with a temperature of 300 ℃, and the inlet temperature was 250 ℃. The carrier gas was nitrogen and the column temperature was programmed. Splitless injection was conducted, and the injection volume was 1 μL. GC-MS was used for the qualitative confirmation of PAEs of samples. Results: The pick area and concentration of six kinds of PAEs showed good linearity (r=0.9994-0.9999). The average recovery rate was 96.8%-100.4% (n=9, RSD ＜3.0%). The PAEs were detected in drugs and the drug packaging materials in the three batches of samples. Conclusion: The method showed good separation and was simple, rapid, sensitive and precise, which was suitable for the simultaneous detection