UPLCMS/MS法同时测定白蒲黄胶囊中12种有效成分

doi:10.3969/j.issn.10073205.2019.01.022

摘要/Abstract

摘要： ［摘要］〓
〖HTH〗目的〖HTSS〗〖KG*2〗建立超高效液相色谱-串联质谱（ultra high performance liquid chromatography tandem mass spectrometry，UPLCESIMS/MS）方法同时测定白蒲黄胶囊中β蜕皮甾酮、筋骨草甾酮C、常春藤皂苷C、刺人参皂苷S、白头翁皂苷C、C47H76O17、白头翁皂苷B4、常春藤皂苷B、白头翁皂苷A3、α常春藤皂苷、23羟基白桦脂酸和常春藤皂苷元12种成分的含量。
〖HTH〗方法〖HTSS〗〖KG*2〗采用Phenomenex KinetexC18色谱柱（100×3 mm，2.6 mm），流动相为甲醇（0.1%甲酸）-水（0.1%甲酸），梯度洗脱，流速0.4 mL/min，柱温40 ℃。采用电喷雾离子源进行正、负离子模式进行检测，多反应监测模式进行定量测定。离子源温度（Source Temp）为150 ℃，毛细管（Capillary）电压为2.0 kV，离子源补偿电压（Source Offset）为50 V，脱溶剂气温度（Desolvation Temp）为500 ℃，雾化气（Nebuliser）压力7.0 Bar，接口处加热。
〖HTH〗结果〖HTSS〗〖KG*2〗在6.5 min内白蒲黄胶囊中12种有效成分β蜕皮甾酮、筋骨草甾酮C、常春藤皂苷C、刺人参皂苷S、白头翁皂苷C、C47H76O17、白头翁皂苷B4、常春藤皂苷B、白头翁皂苷A3、α常春藤皂苷、23羟基白桦脂酸和常春藤皂苷元被完全分离；峰面积与其浓度呈良好的线性；平均回收率范围为97.13%~101.2%，相对标准差为1.2%~4.1%。
〖HTH〗结论〖HTSS〗〖KG*2〗该测定方法经验证分析时间短、专属性高，可为白蒲黄胶囊质量控制提供依据。

关键词: 白蒲黄胶囊, 色谱法, 高压液相, 质量控制

Abstract: ［Abstract］ Objective〖HTSS〗〓To develop a ultra high performance liquid chromatography tandem mass spectrometry(UPLCESIMS/MS) method for the simultaneous determination of 12 compounds(βecdysterone, ajugasterone C, hederasaponin C, cirenshenoside S, pulsatilloside C, C47H76O17, anemoside B4, hederasaponin B, anemoside A3, αhederin, 23hydroxybetulinic acid and hederagenin) in Baipuhuang capsules.
〖HTH〗〖WTHZ〗Methods〖HTSS〗〓The chromatographic separation was performed on a Phenomenex KinetexC18 column (100×3 mm, 2.6 mm) and the column temperature was set at 40 ℃. The mobile phase, 0.1%(v/v) formic acid (A) and methanol consisted of 0.1% formic acid (B), were run at a flow rate of 0.4 mL/min and the analytes were eluted with a gradient system. Multiplereaction monitoring scanning was employed for determination with positive and negative modes. The conditions of MS/MS detector were set as follows: source temperature 150 ℃, capillary voltage 2.0 kV, and desolvation temperature 350 ℃, desolvation and cone gas at a flow rate of 800 and 150 L/h, respectively. Atomization gas pressure 7.0 Bar and the interface heater was turned on.
〖HTH〗〖WTHZ〗Results〖HTSS〗〓The complete separation was obtained within 14 min for the 12 compounds(βecdysterone, ajugasterone C, hederasaponin C, cirenshenoside S, pulsatilloside C, C47H76O17, anemoside B4, hederasaponin B, anemoside A3, αhederin, 23hydroxybetulinic acid and hederagenin). Seven regression equations showing linear relationships between peak area and content of each compound were obtained. The recoveries(n=6) of the compounds were 97.13%-101.2% and relative standard deviation were 1.2%-4.1%, respectively.
〖HTH〗〖WTHZ〗Conclusion〖HTSS〗〓The analytical method established in this study posseses the advantage of simple operation, rapid speed, strong specificity and high sensitivity, and can be employed to the simultaneous quantification of multiple components in Baipuhuang capsules.

Key words: Baipuhuang capsules, chromatography, high pressure liquid； quality control

魏婷婷，金苗苗，甘晓若，马梦含，杨国珍，许慧君*. UPLCMS/MS法同时测定白蒲黄胶囊中12种有效成分[J]. 河北医科大学学报, doi: 10.3969/j.issn.10073205.2019.01.022.

WEI Tingting, JIN Miaomiao, GAN Xiaoruo, MA Menghan, YANG Guozhen, XU Huijun*. Determination of 12 kinds of compounds in Baipuhuang capsules by UPLCMS/MS#br#[J]. Journal of Hebei Medical University, doi: 10.3969/j.issn.10073205.2019.01.022.

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UPLCMS/MS法同时测定白蒲黄胶囊中12种有效成分

Determination of 12 kinds of compounds in Baipuhuang capsules by UPLCMS/MS#br#

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