摘要
目的:建立快速的反相高效液相色谱法同时测定和比较不同产地雷公藤根皮中3种生物碱含量。方法:采用 Microsorb-100 C_(18)反相色谱柱(250 mm×4.6 mm,5 μm),以乙腈和0.02 mol·L^(-1)磷酸二氢钾水溶液作为流动相,分2个梯度进行洗脱:1→8 min 时梯度变化为50:50→70:30,而8→12 min 时70:30→100:0,最后保持乙腈洗脱3 min。进样量10 μL,流速为1mL·min^(-1),检测波长为254 nm,柱温为35℃。结果:在该色谱条件下,雷公藤定碱(wilfordine)、雷公藤吉碱(wilforgine)及雷公藤次碱(wilforine)被成功分离;线性相关性在0.9996~0.9998之间;3种生物碱的加样回收率分别为99.1%,99.9%,98.8%,RSD 分别为0.99%,0.76%,0.64%。结论:用所建立的方法直接测定和比较了浙江、湖北、广西和福建雷公藤根中的3种生物碱含量,分离度高,分析快速、准确。
Objective:To establish a method for the determination of 3 alkaloids in Tripterygium wilfordii root bark by RP- HPLC. Methods:Three constituents were separated on a C18 column (250 mm × 4. 6 mm,5 μm) using acetonitrile and water( containing 0. 02 mol · L^-1 potassium dihydrogen phosphate) as mobile phase, the ratio of two solvent changed from 50:50 to 70:30 in 8 min, then to 100:0 in 4 min, kept the last ratio for 3 min. The flow rate was 1 mL · min^-1, the detection wavelength was 254 nm, and the column temperature was 35 ℃. Results:Wilfordine,wilforgine and wilforine were successfully separated, linear correlation coefficients were between 0. 9996 - 0. 9998 ,the average recoveries of 3 alkaloids were 99. 1% ,99.9% and 98.8% with RSD of 0. 99% ,0. 76% and 0. 64% ,respectively. Conclusion :The contents of wilfordine, wilforgine and wilforine in Tripterygium wilfordii root bark samples collected from different regions were determined. This method is rapid and accurate.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2007年第2期191-193,共3页
Chinese Journal of Pharmaceutical Analysis
基金
浙江省重大项目资助(编号:021102533)
关键词
雷公藤生物碱
雷公藤根皮
反相高效液相色谱
Tripterygium wilfordii alkaloids
Tripterygium wilfordii root bark
RP- HPLC