使用Biotage Isolera快速纯化液相制备色谱进行川芎中洋川芎内酯A和Z藁本内酯的分离提取

2017/08/09   下载量： 15 次

方案摘要

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应用领域 制药/生物制药
检测样本 中药材和饮片
检测项目 含量测定>色谱法
参考标准 SNAP KP-Sil

应用中压柱色谱分离提取川芎中2 个主要内酯类化合物，并对其进行定性检测和结构鉴定。方法: 利用中压柱色 谱分离内酯类化合物，采用120g Biotage SNAP Cartridge KP － C18 － HS 色谱柱，以乙腈－ 0. 5% 醋酸作为中压柱色谱分离的溶 剂体系，流速30 mL·min － 1 ，检测波长280 nm，柱温30 ℃，进样量800 mg;

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方案详情

Separation，extraction and identification of senkyunolide A and

Z － ligustilide in Chuanxiong Rhizoma*

HU Yang，LIU Chun － ming＊＊，HU Yun － mei，MA Bing，ZHANG Yu － chi

( Central Laboratory，Changchun Normal University，Changchun 130032，China)

Abstract Objective: To separate and extract two main lactones from Chuanxiong Rhizoma by medium － pressure

liquid chromatography( MPLC) ，and perform the qualitatively detection and structural identification of the constituents．

Methods: A 120g Biotage SNAP Cartridge KP － C18 － HS column was employed as the separation column;

solvent system of acetonitrile － 0. 5% acetic acid was used for MPLC at the flow rate of 30 mL·min － 1 ; UV detector

was set at 280 nm，and the temperature was 30 ℃; sample volume was 800 mg． The qualitative and quantitative

measurement and structural identification were carried out by high performance liquid chromatography － electrospray

ionization mass spectrometry using a SunFireTM C18 reversed － phase column( 250 mm × 4. 6 mm，5 μm，Waters，

USA) ，the flow rate was 0. 5 mL·min － 1 ． The mass spectrometer was used to scan molecular weight units from m/

z 50 to 1000 with the full scan and positive ion mode，spray voltage was 4. 5 kV，capillary temperature was 250 ℃，

and capillary voltage was 20 V． Results: Two individual compounds senkyunolide A( 11. 3 mg) and Z － ligustilide

( 20. 1 mg) were separated from 800 mg of 60% ethanol extract of Chuanxiong Rhizoma via one － step MPLC separation

with a purity of more than 95%． Conclusion: The MPLC method has the advantages of simpleness and effectiveness

for the separation of senkyunolide A and Z － ligustilide from Chuanxiong Rhizoma．

Key words: medium － pressure liquid chromatography; Chuanxiong Rhizoma; senkyunolide A; Z － ligustilide; lactones;

high performance liquid chromatography － electrospray ionization mass spectrometry; structural identification




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拜泰齐贸易（上海）有限公司
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