UPLC-MS/MS法测定大补阴丸中小檗碱等4种成分含量

目的：建立同时测定大补阴丸中小檗碱、黄柏碱、毛蕊花糖苷、芒果苷的含量方法。方法：采用液质联用技术，以Agilent ZORBAX SB-C18为色谱柱，以甲醇-甲酸铵溶液为流动相，等度洗脱。结果：小檗碱、黄柏碱、毛蕊花糖苷、芒果苷的线性范围分别为5～500 ng·mL-1（r=0.9991）、0.5～50 ng·mL-1（r=0.9994）、1～100 ng·mL-1（r=0.9987）、1.5～150 ng·mL-1（r=0.9990）；加样回收率为98.35%～102.55%，RSD均＜1.60%；平均含量分别为3.55 、0.322、0.511、0.886 mg·g-1。结论：该法专属性强、快速灵敏，可用于大补阴丸中上述4种成分的含量测定。

Simultaneous Determination of 4 Components in Dabuyin Wan by UPLC-MS/MS

Objective: To develop a UPLC-MS/MS method for the determination of berberine, phellodendrine, verbascoside and mangiferin in Dabuyin Wan. Methods: Isocratic elution was carried out with mobile phase consisting of methanol-ammonium formate. The separation was performed on Agilent ZORBAX SB-C18, and the electrospray ionization (ESI) source was tested in both positive and negative ion modes using multiple monitoring (MRM) for analysis of four components. Results: Berberine, phellodendrine, verbascoside and mangiferin were all analyzed exactly, the linear ranges were 5-500 ng·mL-1 (r=0.9991), 0.5-50 ng·mL-1 (r=0.9994), 1-100 ng·mL-1 (r=0.9987), 1.5-150 ng·mL-1 (r=0.9990), respectively. The recoveries of four analytes ranged from 98.35% to 102.55% and the relative standard deviations were all below 1.60%. The average contents of berberine, phellodendrine, verbascoside and mangiferin were 3.55 mg·g-1, 0.322 mg·g-1, 0.511 mg·g-1, 0.886 mg·g-1, respectively. Conclusion: A sensitive, accuracy and suitable UPLC-MS/MS method has been developed, and the method could be applied for the determination of berberine, phellodendrine, verbascoside and mangiferin in Dabuyin Wan.