超高效液相色谱-质谱联用快速同时检测止痒类 - 中国现代应用药学.pdf

超高效液相色谱-质谱联用快速同时检测止痒类中药制剂中添加 11 种 化学药物成分  赵佳丽，欧贝丽，周燕(嘉兴市食品药品检验检测院，浙江 嘉兴 314050) 摘要：目的 建立超高效液相色谱-质谱联用方法快速检测中药制剂中添加的 11 种化学药物成分(马来酸氯苯那敏、氯雷 他定、硝酸咪康唑、盐酸特比萘芬、酮康唑、艾司唑仑、盐酸氯丙嗪、丙酸氯倍他索、醋酸地塞米松、醋酸泼尼松和吲 哚美辛) 。方法 采用 Waters ACQUITY UPLC BEH C18 column(2.1 mm×100 mm ，1.7 µm)；梯度洗脱：流动相 A 为乙 腈，流动相 B 为 5 mmol·L1 乙酸铵(0.1% 甲酸)水溶液。通过比较样品峰与对照品峰的保留时间、一级质谱和二级质谱碎 片离子，确定样品中是否掺杂化学止痒药物。结果 建立的快速超高效液相串联质谱方法检测上述化学药物成分不受药 物辅料干扰，各色谱峰分离良好，11 种待测成分最低检出限为 0.01~0.46 ng·mL1。结论 该方法简便、灵敏度高，可快 速有效地判断中药制剂中是否非法掺入上述化学药品。 关键词：止痒类中药；抗组胺药；抗真菌药；镇静安眠药；糖皮质激素类药；非甾体抗炎药；超高效液相色谱-质谱联用 中图分类号：R917.101 文献标志码：B 文章编号：1007-7693(2016)12-1558-05 DOI: 10.13748/ki.issn1007-7693.2016.12.016 Simultaneous Determination of 11 Chemicals Added in Itching Agents Traditional Chinese edicines by UPLC-MS/MS ZHAO Jiali, OU Beili, ZHOU Yan(Jiaxing Institute for Food and Drug Control, Jiaxing 314050, China) ABSTRACT: OBJECTIVE To develop a method for simultaneous determination of 11 chemicals (chlorphenamine maleate, loratadine, miconazole nitrate, hydrochloric acid terbinafine, ketoconazole, estazolam, chlorpromazine hydrochloride, clobetasol propionate, dexamethasone acetate, prednisone acetate and indomethacin) added illegally in itching agents traditional Chinese medicines(TCMs) by UPLS-MS/MS. METHODS Separation was performed on Waters ACQUITY UPLC BEH C18 column (2.1 mm×100 mm, 1.7 µm), and by gradient elution with acetonitrile and 5 mmol·L1 ammonium acetate aqueous solution (contain 0.1% formic acid ) as the mobile phase. The chemicals detected in samples were identified by comparison of sample peaks with the retention time, mass spectra and the product ions with those of reference substances. RESULTS The developed UPLC-MS/MS method was did not interfered by the adjuvants. The peaks detected could be separated from each other. The ran