摘要:
目的:建立青风藤药材中青藤碱的含量测定方法。方法:青风藤药材粉碎后过筛,取粉末用70%乙醇超声提取,未涂渍熔融石英毛细管(50μm×48.5 cm,有效长度40 cm),以30 mmol/L磷酸二氢钠溶液(水:甲醇=1:4)为缓冲液,运行电压25 kV,温度25℃,内标为盐酸小檗碱,检测波长为210 nm,运行时间20 min。结果:在此条件下青藤碱与内标及其他成分能达到基线分离,青风藤在34.66～346.6μg/mL范围内呈良好的线性关系Y=0.029X-0.03,r=0.999 8,最低检测限为3.466μg/mL(S/N=3),最低定量限为17.33μg/mL(S/N=10),平均加样回收率为100.1%(RSD=3.1%,n=6),低、中、高浓度日内、日间精密度RSD均小于5%(n=3)。结论:此方法可用于青风藤药材中青藤碱的含量测定,具有方法简便快速、准确、试剂消耗量少的优点。
Abstract:
Objective :To establish a method for determination of sinomenine in Caulis Sinomenii. Methods :Caulis Sinomenii was extracted with 70% alcohol after pulverized to powder.An untreated fused-silica capillary(48.5 cm×50μm,40cm effective length) was used,the running buffer was 30 mmol/L sodium acid phosphate,the solvent was water:methanol=14,the voltage was 25 kV,the temperature was 25 ℃,the internal standard was berberine hydrochloride,the ultraviolet wavelength was set at 210 nm,running time was 20 minute. Results :Sinomenine,internal standard and impurities were separated by baseline in above conditions,sinomenine was liner in the range of 34.66～346.6 μg/mL,linear equation was Y=0.029X-0.03,r=0.9998,the correlation was 0.9998,the limit of determination was 3.466 μg/mL(S/N=3),the limit of quantitation was 17.33 μg/mL(S/N=10),the average recovery was 100.1%(RSD=3.1%,n=6),RSD of intra-day and inter-day were lower than 5%(n=3). Conclusion :The method can be utilized for the determination of sinomenine in Caulis Sinomenii,it was the advantages of convenience,fastness,accuracy,low sample and reagent consumption.
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