HPLC-MS法测定知母盐炙前后8种成分量变化  

Determination of eight constituents in Anemarrhenae Rhizoma before and after salt processing by HPLC-MS

作　　者：季德[1,2] 苏晓楠 黄紫炎 张雪荣[1] 陆兔林[1,2] 

机构地区：[1]南京中医药大学药学院,江苏南京210023 [2]江苏省中药炮制重点实验室,江苏南京210023

出　　处：《中草药》2017年第9期1784-1790,共7页Chinese Traditional and Herbal Drugs

基　　金：国家自然科学基金资助项目(81303223);高等学校博士学科点专项科研基金(20133237120007);江苏省高校自然科学研究项目(13KJB360012);江苏省高校优势学科建设工程项目

摘　　要：目的建立HPLC-MS法同时测定知母中新芒果苷、芒果苷、知母皂苷E_1、知母皂苷BⅡ、知母皂苷BⅢ、知母皂苷Ⅰ、知母皂苷AⅡ、知母皂苷AⅢ 8种化学成分量的方法,分析炮制前后各成分量的变化。方法色谱柱为Agilent SB-C_(18)柱(50 mm×2.1 mm,1.8μm),流动相为0.1%甲酸水溶液-乙腈,梯度洗脱,体积流量0.4 mL/min,柱温30℃,进样量10μL。质谱采用大气压电喷雾离子源,选择性负离子模式监测。结果所测定的8种成分在各自的线性范围内均具有良好的线性关系(r≥0.999 7);平均回收率在97.55%~103.01%,RSD<2.80%。不同产地知母8种成分的量差异较大,其中芒果苷、知母皂苷BⅡ、知母皂苷AⅢ的量较高。知母盐炙后新芒果苷、芒果苷、知母皂苷AⅡ、知母皂苷AⅢ量变化不明显,知母皂苷E_1、知母皂苷BⅡ、知母皂苷Ⅰ量下降,知母皂苷BⅢ量上升。结论该方法简单、灵敏、准确,知母盐炙前后多种成分量发生变化。Objective To establish an HPLC-MS method for the simultaneous quantitation of neomangiferin, mangiferin, timosaponin E_1, timosaponin BⅡ, timosaponin BⅢ, anemarrhenasaponin Ⅰ, timosaponin AⅢ, and timosaponin AⅡ in Anemarrhenae Rhizoma, and to analyze the content change before and after salt processing. Methods Chromatography was performed on Agilent SB-C18（50 mm × 2.1 mm, 1.8 μm） column by gradient elution using 0.05% formic acid in water（A）-acetonitrile（B） at the flow rate of 0.4 mL/min. The column temperature was kept at 30 ℃ and the inject volume was 10 μL. HPLC-MS was used for quantification in negative ion mode under ESI. Results The eight components had good linearity（r ≥ 0.9997） within the linear range. The average recovery rate was 97.55%—103.01% with RSD 〈2.80%. The contents of the eight components in Anemarrhenae Rhizoma varied according to the different habits. The contents of mangiferin, timosaponin BⅡ, and timosaponin AⅢ were high. After salt processing, contents of timosaponin E_1, timosaponin BⅡ, and anemarrhenasaponin Ⅰ were reduced, content of timosaponin BⅢ was increased and contents of neomangiferin, mangiferin, timosaponin AⅢ, and timosaponin AⅡ had no obvious changes. Conclusion The changes of components in Anemarrhenae Rhizoma before and after salt processing are proved by the method of HPLC-MS which is simple, sensitive, and accurate.

关 键 词：知母 盐炙 HPLC-MS 新芒果苷 芒果苷 知母皂苷E1 知母皂苷BⅡ 知母皂苷BⅢ 知母皂苷Ⅰ 知母皂苷AⅡ 知母皂苷AⅢ 

分 类 号：R283.1[医药卫生—中药学]