UHPLC-MS/MS同时测定黄芩清热除痹胶囊中6种活性成分

Simultaneous Determination of Six Active Components in Huangqin Qingre Chubi Capsule by Ultra-high-performance Liquid Chromatography-Tandem Mass Spectrometry

目的建立超高效液相色谱-串联质谱同时测定黄芩清热除痹胶囊中6种成分(黄芩苷、栀子苷、木犀草素、齐墩果酸、薏苡素、苦杏仁苷)含量的方法。方法采用Phenomenex Luna Omega C_(18)色谱柱(100 mm×2.1 mm,1.6μm),以含10 mmol/L甲酸铵的0.1%甲酸水溶液(A)-0.1%甲酸的乙腈(B)为流动相,进行梯度洗脱,柱温为30℃,流速为0.25 mL/min,进样量5μL,分析时间10 min。采用电喷雾离子源,以多反应监测模式在负离子条件下进行检测。结果所测6种活性成分在测定浓度范围内线性关系良好(r≥0.9990),精密度、稳定性和重复性良好,平均加样回收率为98.62%~103.7%,RSD≤2.70%。结论该方法准确度高、分析速度快、检测限低、重复性高,适用于黄芩清热除痹胶囊质量控制。

Objective To establish a method of ultra-high-performance liquid chromatography-tandem triple quadrupole mass spectrometry(UHPLC-MS/MS)in the simultaneous determination of six active components(baicalin,geniposide,luteolin,oleanolic acid,coixol,and amygdalin) in Huangqin Qingre Chubi Capsule. Methods UHPLC-MS/MS was performed on a Phenomenex Luna Omega C 18 column (100 mm×2.1 mm, 1.6 μm) with a mobile phase of 0.1% formic acid solution containing 10 mmol/L ammonium formate (A)-acetonitrile with 0.1% formic acid (B) for gradient elution,at a column temperature of 30 ℃,a flow rate of 0.25 mL/min,a sample size of 5 μL,and an analysis time of 10 minutes. Electrospray ionization source was used for determination in the multiple reaction monitoring mode under anion conditions. Results The above six active components showed a good linear relationship within the range of concentration determined ( r ≥0.999 0) and had good precision,stability,and reproducibility,with an average recovery rate of 98.62%-103.7%(relative standard deviation ≤2.70%). Conclusion This method has high accuracy, rapid analysis speed,low limit of detection,and high reproducibility and is thus suitable for the quality control of Huangqin Qingre Chubi Capsule.