摘要
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SunFireTMC18(250 mm×4.6 mm,5μm)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 constitu- ents. 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 detec- tor 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 （250mm×4.6mm,5μm, 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 sepa- ration with a purity of more than 95%. Conclusion： The MPLC method has the advantages of simpleness and effec- tiveness for the separation of senkyunolide A and Z - ligustilide from Chuanxiong Rhizoma.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2013年第1期69-72,共4页
Chinese Journal of Pharmaceutical Analysis
基金
国家自然科学基金项目(30970299)
国家自然科学基金资助项目(31170326)
关键词
中压柱色谱
川芎
洋川芎内酯A
Z-藁本内酯
内酯类化合物
高效液相色谱-电喷雾质谱联用
结构鉴定
medium - pressure liquid chromatography
Chuanxiong Rhizoma
senkyunolide A
Z - ligustilide
lac-tones
high performance liquid chromatography- electrospray ionization mass spectrometry
structural identification
