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目的:建立高效液相色谱串联质谱法(LC-MS-MS)测定知母黄柏药对中芒果苷、新芒果苷、知母皂苷AⅢ和知母皂苷BⅡ的含量,研究不同配伍比例对4种成分含量的影响。方法:采用ZORBAX Eclipse XDB-C_(18)色谱柱(2.1 mm×150 mm,3.5μm),柱温30℃,流动相0.1%甲酸水-乙腈,流速0.25 m L·min~(-1),梯度洗脱;质谱条件为电喷雾(ESI)离子源,负离子多反应离子监测(MRM)用于定量测定。结果:芒果苷、新芒果苷、知母皂苷AⅢ和知母皂苷BⅡ分别在5.05~404,5.3~424,5.05~404,20.8~1 664μg·L~(-1)线性关系良好(r≥0.999);平均回收率分别为100.6%,99.2%,99.1%,98.5%。知母单煎时芒果苷、知母皂苷AⅢ含量最高;新芒果苷在知柏配伍比例1∶1时含量最高;知母皂苷BⅡ的含量各配伍比例没有明显差异。结论:该方法快速、准确,适用于知母黄柏中4种成分的含量测定。知母与黄柏配伍比例不同,芒果苷、新芒果苷、知母皂苷AⅢ的含量不同,配伍黄柏时对知母成分含量有影响。
OBJECTIVE: To establish a HPLC-MS-MS method for the determination of midrange mangiferin, neogeninoside, timosaponin AⅢ and timosaponin BⅡ in Zhimu, Effect of ingredient content. METHODS: The mobile phase consisted of 0.1% formic acid in water and acetonitrile at a flow rate of 0.25 mL · L -1 on a ZORBAX Eclipse XDB-C 18 column (2.1 mm × 150 mm, 3.5 μm) Gradient elution; mass spectrometry conditions for the electrospray ionization (ESI) ion source, anion multi-reactive ion monitoring (MRM) for quantitative determination. Results: The linear relationships between mangiferin, ne mangiferin, timosaponin A and timosaponin B II were good at 5.05 ~ 404,5.3 ~ 424,5.05 ~ 404,20.8 ~ 1664μg · L ~ (-1) (r≥0.999 ). The average recoveries were 100.6%, 99.2%, 99.1% and 98.5% respectively. The results showed that mangiferin and timosaponin AⅢhad the highest content when there was a single decoction. The content of ne mangiferin was the highest when the compatibility ratio was 1: 1. The content of timosaponin BⅡwas not significantly different among different proportions. Conclusion: The method is rapid and accurate and is suitable for the determination of four components in. Anemarrhena and cortex phellodendri compatibility proportion of different mangiferin, ne mangiferin, timosaponin A Ⅲ different content, compatibility cork when the Zhimu ingredients affect.