基于液相色谱-串联质谱法的养阴清肺丸中麦冬投料情况研究

Study on the Feeding Situation of Ophiopogonis Radix in Yangyin Qingfei Pills by HPLC-MS/MS

目的:建立养阴清肺丸中同时测定甲基麦冬黄烷酮A、甲基麦冬黄烷酮B、山麦冬皂苷B和短葶山麦冬皂苷C的分析方法,判断麦冬的投料情况。方法:应用高效液相色谱-三重四极杆串联质谱(HPLC-MS/MS)技术,采用Agilent Poroshell 120 EC-C18(3.0 mm×100 mm,2.7μm)色谱柱,以乙腈-0.1%甲酸溶液为流动相,流速0.3 mL·min^(-1),柱温35℃,进样量5μL;采用电喷雾离子源(ESI),正、负离子2种模式,以多反应监测模式(MRM)进行分析。结果:4个成分在相应的范围内线性关系良好(r>0.9991),平均回收率为96.61%~98.65%。59批养阴清肺丸样品中有39批存在以山麦冬替代或者混入麦冬投料问题。结论:建立的方法简单、准确、可靠,可用于判断养阴清肺丸中麦冬的投料情况及市场监管。

Objective: To establish a method for the simultaneous determination of Methylophiopogonanone A,Methylophiopogonanone B, Liriopesides B and Liriopemuscari baily saponins C in Yangyin Qingfei pills and determine the feeding situation of Ophiopogonis Radix. Methods: The high performance liquid chromatographytriple quadruple mass spectrometry(HPLC-MS/MS) was performed on an Agilent Poroshell 120 EC-C18column(3.0 mm × 100 mm, 2.7 μm) with mobile phase consisting of acetonitrileand 0.1% aqueous formic acid. The flow rate was controlled at 0.3 mL·min^(-1), and the column temperature was set at 35 ℃, and the sample volume was 5 μL. A mass spectrometer equipped with electrospray ionization source was used as detector operated in positive and negative ion mode. Multiple reaction monitoring(MRM) was performed. Results: Four components showed good linear correlation within their ranges(r>0.9991), and the averaged recoveries ranged from 96.61% to 98.65%. In the 59 batches of Yangyin Qingfei pills, 39 batches had the feeding problem of using Liriopes Radix instead of Ophiopogonis Radix or mixing in Ophiopogonis Radix. Conclusion: The established method is simple, accurate, reliable, and could be used in the determination of the feeding situation of Ophiopogonis Radix in Yangyin Qingfei pills and market regulation.