保健酒及酒类制品中非法添加PDE-5抑制剂及其衍生物的监测及结果分析

发布时间：2018-04-21 16:53

本文选题：保健酒及酒类制品 + PDE-抑制剂及其衍生物　；参考：《药物分析杂志》2017年02期

【摘要】：目的:对保健酒及酒类制品中非法添加磷酸二酯酶(PDE-5)抑制剂及其衍生物进行监测,并对监测结果进行分析讨论。方法:参照"国家食品药品监督管理局药品检验补充检验方法和检验项目批准件(编号2009030)方法。LC-MS/MS法条件:采用Shim-pack XR-ODS(100 mm×2.0 mm,2.2μm)色谱柱,以0.1%乙酸的10 mmol·L~(-1)乙酸铵溶液(A)-乙腈(B)为流动相,梯度洗脱(0~8 min,27%B;8~18 min,27%B→80%B,18~20 min,80%B),流速0.3 m L·min~(-1);采用电喷雾离子源(ESI),正离子扫描模式,一级质谱全扫描范围为m/z 100~1 000,二级质谱全扫描范围为m/z 40~1 000。HPLC法条件:采用Inertsil ODS-SP C18(4.6 mm×150 mm,5μm)色谱柱,以10 mmol·L~(-1)乙酸铵溶液(A)-甲醇(B)-乙腈(C)为流动相,梯度洗脱(0~15 min,10%B→25%B;15~25 min,25%B→55%B;25~35 min,55%B,保持15%C),流速1.0 m L·min~(-1),柱温为室温,二极管阵列检测器,扫描范围为200~400 nm。结果:64批次样品中12批次检测到PDE-5抑制剂及其衍生物,其中检出批件中涉及的西地那非、伐地那非、氨基他达拉非和羟基豪莫西地那非4种非法添加成分。另外检出5种批件中未涉及的PDE-5抑制剂衍生物,为丙氧基苯基艾地那非、丙氧基苯基硫代艾地那非、艾地那非和羟基硫代豪莫西地那非,且有一种未见报道的新型PDE-5抑制剂衍生物(暂无命名)。结论:保健酒及酒类制品中检出非法添加PDE-5抑制剂及其衍生物,需建立快速有效的针对新型PDE-5衍生物的监测方法,并加强对相关销售渠道的监管,保障人民生命健康。
[Abstract]:Objective: to monitor the illegal addition of phosphodiesterase (PDE-5) inhibitor and its derivatives in health wine and its products, and analyze the results. Methods: referring to the method of supplementary inspection for drug inspection of the State Food and Drug Administration (SFADA) and the method of item approval (No. 2009030). LC-MS / MS method: the chromatographic column of Shim-pack XR-ODS(100 mm 脳 2.0 mm ~ (2. 2 渭 m) was used, and the mobile phase was 10 mmol / L ~ (-1) ammonium acetate solution with 0.1% acetic acid as the mobile phase. The mobile phase was 10 mmol / L ~ (-1) ammonium acetate solution, and the gradient elution was 10 ~ (15) min ~ (-1) and 10 ~ (25) min ~ (25) B ~ (5) B ~ (55) B ~ (55) B ~ (55) B ~ (25) 25 ~ (35) min ~ (55) ~ (55) B, keeping 15C, flow rate was 1.0 mL / min ~ (-1), column temperature was room temperature, diode array detector was used, scanning range was 200 ~ (400) nm. Results PDE-5 inhibitors and their derivatives were detected in 12 of the 12 batches of w 64 batches of samples. Four kinds of illegal additives were detected, including sildenafil, vardenafil, aminotadalafil and hydroxyl Homoscindinafil. In addition, the PDE-5 inhibitor derivatives not involved in the five batches were found to be propoxyl phenyl idenafil, prooxy phenyl thioethylenafil, aldenafil and hydroxyl thiohamosildenafil. And there is a new type of PDE-5 inhibitor derivative that has not been reported. Conclusion: it is necessary to establish a rapid and effective method for monitoring the new type of PDE-5 derivatives and strengthen the supervision of the relevant sales channels to protect the people's life and health by detecting the illegal addition of PDE-5 inhibitors and their derivatives in health wine and liquor products.
【作者单位】：河北省药品检验研究院;
【基金】：河北省食品药品监督管理局2014年度食品药品安全科技项目重点项目(ZD2014006)
【分类号】：R155.5

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