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目的:采用液相色谱-二极管阵列-串联质谱检测法(LC-DAD-MS/MS)定性、定量检测某抗风湿中药中非法添加的双氯芬酸盐。方法:选用Agilent ZORBAX SB C_(18)(150 mm×4.6 mm,5μm)柱,以甲醇-20 mmol·L~(-1)乙酸铵溶液(60:40)为流动相,对非法制剂的提取液进行分析。通过与对照品的色谱保留时间、紫外吸收光谱及质谱碎裂行为的比较,对此类药进行定性鉴别和定量测定。结果:某抗风湿中药胶囊剂两个批次均检测到了西药双氯芬酸盐。结论:所用方法专属性强、灵敏度高、操作简便,可作为分析中药中非法添加双氯芬酸盐的参考方法。
OBJECTIVE: To qualitatively and quantitatively detect diclofenac illegally added to an anti-rheumatoid drug by liquid chromatography-diode array-tandem mass spectrometry (LC-DAD-MS / MS) Methods: An Agilent ZORBAX SB C 18 column (150 mm × 4.6 mm, 5 μm) was used as the mobile phase. The mobile phase was methanol-20 mmol·L -1 ammonium acetate solution (60:40) Liquid for analysis. By comparing the chromatographic retention time, UV absorption spectra and mass spectrum fragmentation with the reference substance, qualitative identification and quantitative determination of such drugs. Results: Western medicine diclofenac was detected in two batches of one anti-rheumatoid medicine capsule. Conclusion: The method used is specific, sensitive and easy to operate. It can be used as a reference method for the analysis of illegal addition of diclofenac in traditional Chinese medicine.