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目的:建立同时测定白蒲黄片中7种五环三萜皂苷类成分白头翁皂苷A3、白头翁皂苷B4、23-羟基白桦脂酸、白头翁皂苷B、白头翁皂苷C、刺人参苷S和齐墩果酸的HPLC-MS法。方法:采用Diamonsil ODS C18(250 mm×4.6 mm,5μm)色谱柱,流动相为含0.1%甲酸的水(A)-含0.1%甲酸的甲醇(B),梯度洗脱程序为25%A(0 min),5%A(0~6 min),5%A(6~14min),25%A(保持6 min),流速0.8 m L·min-1,柱温30℃,进样量10μL;采用正离子和负离子模式同时监测,正离子和负离子监测模式下源喷射电压分别为5.5 k V和-4.5 k V,离子源温度为650℃,雾化气(Gas 1)344 k Pa,加热气(Gas 2)412 k Pa,接口持续加热,帘气172 k Pa,全程氮气通入状态。结果:在14 min内白蒲黄片中7种有效成分白头翁皂苷A3、白头翁皂苷B4、23-羟基白桦脂酸、白头翁皂苷B、白头翁皂苷C、刺人参苷S和齐墩果酸被完全分离;峰面积与其浓度呈良好的线性;平均回收率范围为95.11%~107.3%,RSD为0.86%~3.26%。结论:本文建立的方法经验证简便、重现性好、专属性高,可为白蒲黄片质量控制提供参考。
Objective: To establish a method for the simultaneous determination of seven pentacyclic triterpene saponins Pulsatilla saponin A3, Pulsatilla saponin B4,23-hydroxy betulinic acid, Pulsatilla saponin B, Pulsatilla saponin C, ginsenoside S and oleanolic acid HPLC-MS method. METHODS: Diamonsil ODS C18 column (250 mm × 4.6 mm, 5 μm) was used. The mobile phase consisted of 0.1% formic acid in water (A) and 0.1% formic acid in methanol (0 min), 5% A (0-6 min), 5% A (6-14 min), 25% A for 6 min and the flow rate was 0.8 m L · min-1. ; Simultaneous monitoring with both positive and negative ion modes, with source voltages of 5.5 kV and -4.5 kV for positive and negative ion monitoring modes, 650 ° C for the ion source, 344 kPa for Gas 1, heating Gas 2 412 k Pa, continuous heating of the connection, curtain air 172 k Pa, full nitrogen feed-in. Results: Within 14 min, Pulsatilla saponin A3, Pulsatilla saponin B4,23-hydroxy betulinic acid, Pulsatilla saponin B, Pulsatilla saponin C, ginsenoside S and oleanolic acid were completely separated from Baipuweng tablet. The peak area and its concentration showed a good linearity. The average recoveries ranged from 95.11% to 107.3% with RSDs ranging from 0.86% to 3.26%. Conclusion: The method established in this paper is simple, reproducible, highly specific and can provide reference for the quality control of Bai Puhuang tablets.