液质联用技术对保健品中添加西药分的检测.doc

天津中医药大学中药学院 2005级本科生毕业论文 液质联用技术对保健品中添加西药成分的检测 专 业： 中药学 姓 名： 彭友明 指导教师： 朱小兰 天 津 中 医 药 大 学 2009年6月 液质联用技术对保健品中添加 西药成分的检测 中药学院　　2005级中药学2班 彭友明 指导教师 朱小兰 工程师 摘 要 摘要 目的:建立LC-MS/MS甄别保健品中可能添加的西药成分的方法。方法：采用C18色谱柱，梯度洗脱：流动相A为乙腈溶液，流动相B为水（含0.2%甲酸，5mmol醋酸铵），波长扫描范围为220-340m，流速为1mL/min。选择正负离子同时扫描方式检测。结果：通过分子量、质谱碎片信息和在液相色谱上的保留特征,初步判断保健品里掺有的西药成分双氯芬酸钠和布洛芬，通过与对照品的分析对比进行了确证，并对其含量进行了测定。结论：该方法选择性强,灵敏度高,可作为分析检测在保健品中添加西药成分的有效方法。 关键词: 保健品；双氯芬酸纳；布洛芬； LC-MS/MS　 Identification and Determination of Illegal Medicament Added in Health Care Products by LC-MS/MS Abstract Objective: To develop a high performance liquid chromatography - electro-spray mass spectrometry method for identifying illegally adulterated in Health Care Products. Methods: A Cl8 column was used with the mobile phase acetonitrile and water（contains 0.2％ formic acid and 5mmol Ammonium acetate）by gradient elution, the detection wavelength was 220-340nm, the flow rate was l mL/min. Electro-spray ionization (ESI) source was applied and operated in the positive and negative ion mode. Results: Using the method, two compounds - Diclofenac Sodium and Ibuprofen had been detected. Also their content had been determined. Conclusion: The method is accurate, simple and sensitive, and it can be used for determination the illegal medicament which added in Health Care Products. Keywords : Health Care Products; Diclofenac Sodium; Ibuprofen; LC-MS/MS 目 录 绪言……………………………………………………………………………………………1 液质联用技术对保健品中添加西药成分的检测 1材料与方法……………………………………………………………………………………2 1.1 仪器和试剂………………………………………………………………………………2 1.2 色谱条件…………………………………………………………………………………2 1.3 质谱条件…………………………………………………………………………………2 1.4 标准溶液的配制…………………………………………………………………………3 1.5 样品处理………………………………………………………………………………… 3 2结果……………………………………………………………………………………………4 2.1 药物组分的确认…………………………………………………………………………4 2.2 提取工艺的优化…………………………………………………………………………8 2.3 线性实验………………………………………………………………………………… 9 2.4 精密度实验……………………………………………………………………………10 2.5 回收率实验………………………………………………………………………………11 2.6 药物含量测定………………………