UPLC-MS/MS法测定茯苓、茯苓皮和茯神中茯苓新酸B、去氢土莫酸、猪苓酸C、去氢茯苓酸和茯苓酸

Determination of poricoic acid B,dehydrotumulosic acid,polyporenic acid C,dehydropachymic acid,and pachymic acid in Poria,Poria peel,and Poria with hostwood by UPLC-MS/MS

目的建立超高效液相色谱串联质谱(UPLC-MS/MS)法同时测定茯苓、茯苓皮和茯神中茯苓新酸B、去氢土莫酸、猪苓酸C、去氢茯苓酸和茯苓酸。方法采用Shim-pack GIST C18AQ色谱柱(100 mm×2.1 mm,3μm),以乙腈–0.1%甲酸为流动相,梯度洗脱,体积流量0.4 mL/min,柱温40℃,进样量5μL。质谱采用离子源:ESI,负离子模式采集,采集模式:多反应监测(MRM),离子源温度150℃,毛细管电压2.5 kV,锥孔电压40 V,去溶剂气流量900 L/h,去溶剂气温度500℃。结果茯苓新酸B、去氢土莫酸、猪苓酸C、去氢茯苓酸和茯苓酸在各自的线性范围内线性关系良好,平均回收率分别为97.80%、99.65%、97.32%、102.82%、99.57%,RSD值分别为3.46%、1.29%、3.01%、3.11%、1.89%。茯苓皮中5种三萜类成分含量均高于茯苓和茯神。结论本法具有分析速度快、准确度高的优点,可为茯苓、茯苓皮和茯神的质量标准提高和开发利用提供依据。

Objective To establish an UPLC-MS/MS method for simultaneous determination of poricoic acid B,dehydrotumulosic acid,polyporenic acid C,dehydropachymic acid,and pachymic acid in Poria,Poria peel,and Poria with hostwood.Methods Shimpack GIST C18AQ column(100 mm×2.1 mm,3μm)was used with acetonitrile-0.1%formic acid as the mobile phase by gradient elution.The flow rate was 0.4 mL/min,the column temperature was 40℃,and the injection volume was 5μL.Mass spectrometry adopted the following conditions:ion source:ESI,negative ion mode collection,collection mode:multi-reaction monitoring(MRM),ion source temperature 150℃,capillary voltage 2.5 kV,cone voltage 40 V,desolvent gas flow 900 L/h,and desolvent gas temperature 500℃.Results Poricoic acid B,dehydrotumulosic acid,polyporenic acid C,dehydropachymic acid,and pachymic acid showed good linear relationship within their linear range.The average recoveries were 97.80%,99.65%,97.32%,102.82%,and 99.57%with RSD values of 3.46%,1.29%,3.01%,3.11%,and 1.89%.The content of five triterpenoids in Poria peel was higher than those in Poria and Poria with hostwood.Conclusion This method has the advantages of fast analysis speed and high accuracy,and can provide a basis for the improvement of the quality standard and the development and utilization of Poria,Poria peel,and Poria with hostwood.