非法添加止咳平喘类药物中药制剂的HPLC-MS/MS检测系统研究

目的: 建立准确、灵敏的HPLC-MS/MS方法检查中药制剂及保健食品中非法添加的14种化学合成止咳平喘药物。 方法: 采用Ultimates^TM XB-C₁₈(4.6 mm×150 mm,5 μm)色谱柱,梯度洗脱:流动相A为20 mmol·L^-1醋酸铵溶液(用氨水调pH至9.0),流动相B为甲醇,检测波长为230 nm,流速为1 mL·min^-1(分流比4∶ 1)。正负离子检测茶碱、二羟丙茶碱、羟乙基茶碱、多索茶碱、盐酸克仑特罗、氯丙那林、二氧丙嗪、氢溴酸右美沙芬、盐酸氨溴索、硫酸沙丁胺醇、盐酸丙卡特罗、磷酸可待因、盐酸班布特罗、富马酸酮替芬,扫描方式采用全扫描一级质谱、全扫描二级质谱(MS²),质荷比范围100~1000。 结果: HPLC-MS/MS方法测定上述化学物质的最小检出量为4~80 ng。 结论: 该方法建立的系统能够灵敏、准确地测定中药中非法添加止咳平喘类药物。

Objective: To establish an HPLC-MS/MS method for separation and identification antitussives which added illegally in Chinese medicine.A method for the analysis of antitussives in Chinese medicine and Heath Food was developed by high performance liquid chromatography electrospray ion trap mass spectrometry (Finnigan LCQ). Methods: The fragmentation pattern of these drugs was summarized.After separated by HPLC,the organic solvent extraction from traditional Chinese medicine preparations was analyzed by the mass spectrometer,operated in positive ion or negative mode and in three scan modes including full scan MS,selected ion monitoring and full scan MS².The obtained pseudomolecular ions and fragment ions were used to identify these drugs. Results: HPLC and MS resolution of above antitussives were good. Conclusion: The method offers advantages of specificity,speed and sensitivity.