地黄炮制前后化学成分的UHPLC-Q-TOF/MS比较研究  

Comparison of Chemical Constituents of Crude and Processed Products of Rehmannia glutinosa by Using UHPLC-Q-TOF/MS

作　　者：陶益[1] 蒋妍慧 唐克建 李伟东[1] 蔡宝昌[1] 

机构地区：[1]南京中医药大学中药炮制重点实验室,江苏南京210023

出　　处：《中药新药与临床药理》2016年第1期102-106,共5页Traditional Chinese Drug Research and Clinical Pharmacology

基　　金：江苏省自然科学基金青年项目(BK20140963);科技部"国家科技重大专项"资助项目(2012ZX09304005)

摘　　要：目的比较地黄生品、酒品、蒸制品各项质控指标及化学成分的差异。方法按照中国药典2010版标准,测定地黄不同炮制品的水分、总灰分、醇溶性浸出物,并建立HPLC方法比较地黄不同炮制品主要化学成分的差异,考察方法的线性、精密度、稳定性、重复性及加样回收率,同时使用超高效液相色谱-四极杆飞行时间串联质谱法(UHPLC-Q-TOF/MS)鉴定地黄不同炮制品的主要差异化学成分。结果地黄酒品和蒸品的水分分别为6.06%和10.02%,总灰分分别为6.70%和6.47%,酸不溶性灰分分别为2.63%和2.39%,水溶性浸出物分别为72.62%和77.81%,测定结果均符合中国药典2010版的要求。运用高分辨质谱鉴定了8个主要差异化学成分,即连翘酯苷E、洋地黄叶苷B、焦地黄苯乙醇苷A1、毛蕊花糖苷、异麦角甾苷、连翘酯苷、焦地黄苯乙醇苷D和地黄苷。结论地黄经炮制后梓醇含量显著上升,而其他主要化学成分的含量显著降低,这可能是不同炮制品临床功效存在差异的主要原因。Objective To compare the quality control indexes and chemical constituents of crude and processed Rehmannia glutinosa. Methods According to criteria issued in Chinese Pharmacopoeia 2010 version, the water content,total ash,acid-insoluble ash and water soluble extract of different processed products were detected. HPLC method was used for comparing the contents of major constituents of rude Rehmannia glutinosa and its different processed products. The linearity, precision, stability, repeatability and recoveries of the method were validated.Moreover, ultra-high-performance liquid chromatography-quadrupole-time-of-flight mass spectrometry（UHPLC-QTOF/MS） was also employed to identify major constituents of processed Rehmannia glutinosa products. Results The contents,of water total ash,acid-insoluble ash and water-soluble extract of wine-processed and steamed Rehmannia glutinosa were 6.06 % and 10.02 %, 6.70 % and 6.47 %, 2.63 % and 2.39 %, 72.62 % and 77.81 %,respectively,which were in line with the requirements of the Chinese Pharmacopoeia 2010 edition. Eight components were confirmed as the different constituents from the crude and processed Rehmannia glutinosa by high-solution mass spectrometer,and they were forsythoside E,purpureaside B,jionoside A1,acteoside,isoacteoside,forsythiaside,jionoside D, and martynoside. Conclusion After processing, the content of catalpol of Rehmannia glutinosa was significantly increased, while the contents of other major constituents were decreased significantly, which may be responsible for the different clinical efficacy of various processed products.

关 键 词：地黄 生品 酒品 蒸制品 超高效液相色谱-四极杆飞行时间串联质谱法 

分 类 号：R284.1[医药卫生—中药学]