川芎中洋川芎内酯A和Z-藁本内酯的分离提取及鉴定

目的: 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;利用高效液相色谱-电喷雾质谱联用技术进行定性检测和结构鉴定,采用SunFire^TM C₁₈(250 mm×4.6 mm,5 μm)反相色谱柱,流速0.5 mL·min^-1,正离子模式电喷雾电离,扫描范围m/z 50～1000,喷雾电压4.5 kV,金属毛细管温度250 ℃,金属毛细管电压20 V。结果: 应用中压柱色谱技术一次性从800 mg川芎的60%乙醇提取物中分离得到2个单体化合物,洋川芎内酯A(11.3 mg)和Z-藁本内酯(20.1 mg),其纯度均达到95%。结论: 应用中压柱色谱分离川芎中单体化合物洋川芎内酯A和Z-藁本内酯的方法简单、快捷。

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 SunFire^TM 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.

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