骨通贴膏指纹图谱及化学成分研究

HPLC fingerprint and chemical constituents of Gutong Plaster

目的应用HPLC法建立骨通贴膏(丁公藤、麻黄、当归、干姜等)指纹图谱并结合两种LC/MS联用技术进行多成分结构鉴定。方法以AlltimaTMC18(4.6 mm×250 mm,5μm)为分析柱,0.1%甲酸水溶液-乙腈为流动相,梯度洗脱,检测波长为280nm;质谱定性采用飞行时间质谱(TOF-MS)结合离子阱多级质谱(Ion-trap/MSn),正、负两种离子模式扫描。结果以Z-藁本内酯为参照物峰,确定了骨通贴膏HPLC指纹图谱,指定了19个共有峰(21个化学成分),10批骨通贴膏HPLC指纹图谱相似度大于0.990。结论所建立骨通贴膏指纹图谱分析方法简单准确,稳定可靠,可用于其质量评价。

AIM To establish a fingerprint method for analyzing Gutong Plaster （Erycibes Caulis, Ephedrae Herba, Angelicae sinensis Radix, Zingiberis Rhizoma, etc） by HPLC and a combinative LC/MS method for the identification of multi-components in Gutong Plaster. METHODS An HPLC in combination with PDA detector was applied on AlhimaTM Cls （4.6 mm ×250 mm, 5 μm） column in gradient elution manner using acetonitrile - 0. 1% formic acid solution as the mobile phase. The flow rate was 1 mL/min and the detection wavelength was set at 280 nm. A combination of time-of-flight mass spectrometer （TOF-MS） and ion trap tandem mass spectrometer （Trap-MS＇1） was used for qualitative analysis under positive and negative ion modes. RESULTS HPLC finger- print of Gutong Plaster was established choosing Z-Ligustilide peak as the reference peak and nineteen common peaks （21 chemical constituents） were obtained from standard fingerprint chromatograms of ten batches with simi- larity no lower than 0. 990. CONCLUSION The HPLC method with good precision and reproducibility can be used for the quality control of Guton Plaster.