HPLC/MS/MS法检测中药制剂中解热镇痛及糖皮质激素类化学药

目的: 建立解热镇痛及糖皮质激素等化学药,包括双氯芬酸、萘普生、吲哚美辛、氨基比林、泼尼松及醋酸泼尼松的液相色谱-质谱联用分析方法,为鉴定中药制剂中非法掺入的上述化学药提供检测手段。 方法: 液相部分,采用Agilent C₁₈(150 mm×4.6 mm,5 μm),以0.01 mol·L^－1甲酸铵溶液含0.1%甲酸为流动相A,以甲醇为流动相B,进行梯度洗脱;质谱部分,Agilent离子阱质谱仪,采用一级、二级质谱全扫描方式,同时对双氯酚酸等六种化学药进行色谱分离及质谱鉴定,研究了这六种药物的质谱裂解规律。 结果: 根据化合物的色谱保留时间及一级、二级质谱信息,并与对照品比较,证明被检测的中药制剂中非法掺入了萘普生、双氯芬酸、吲哚美辛。 结论: 该方法选择性强,灵敏度高,可作为分析检测非法中药制剂的有效手段。

Objective: To develop a specific,sensitive and rapid HPLC-MS-MS assay for diclofenac,naproxen,indometacin,amidopyrin,prednisone and prednisone acetate,and provide a detection method for identification of the above chemical drugs illegally adulterated in traditional Chinese medicine(TCM) preparations. Methods: HPLC-MS/MS was used to separate and identify the above chemical drugs. The separation was performed on a Agilent C₁₈(,150 mm×4.6 mm,5 μm) and consisted of 0.01 mol·L^－1ammonium formate(with 0.1% formaic acid)-methanol. The mass spectrometer(Agilent Trap Mass) was operated in the positive ion mode and in two scan modes including full scan MS and full scan MS-MS. The obtained mass spectra were analyzed for their fragmentation passways. Results: The obtained mother ions,fragment ions and retention time were used to identify the above drugs. It was found that naproxen,diclofenac and indometacin were illegally adulterated in the pure TCM preparation. Conclusion:The method is seclective,sensitive and can be used to detect the illegally added components in traditional Chinese preparation and control the quality.