摘要
目的建立测定藏药镰形棘豆中球松素含量的反相高效液相色谱法，从而为控制镰形棘豆的质量提供参考。方法使用Agilent Zorbax Eclipse XDB—Q液相色谱柱（5μm，4．6mm×150mm）；流动相为0．1％甲酸水溶液（A）-乙腈（B），梯度洗脱程序为0～50min，A由75％降至50％，50～60min，A由50％降至40％，60-65min，A由40％升至75％，65～70min，A保持75％；流速为1．0mL／min；检测波长为280nm；柱温为20℃；进样量为5μL。结果样品中的球松素可以与各干扰组分达到基线分离；用本法测定球松素的线性范围为0．101～0．707μg；重复性实验RSD=1.27％（n=5）；平均回收率达到98.2％（n=5），RSD=1.89％；试验中测得样品中球松素的含量为0．16％。结论本方法具有供试品溶液制备简便，重复性好等优点。
OBJECTIVE To establish the reversed phase high-performance liquid chromatography for determination of the content of pinostrobin in the Tibetan drugfalcate crazyweed, so as to provide evidence for the quality control of fa/cate crazyweed.METHOD Agilent Zorbax Eclipse XDB-C8 liquid chromatographic column （5 μm, 4.6 mm× 150 ram） was used, with mobile phase at 0.1% water solution of formic acid （A） acetonitrile （B）, gradient elution at 0- 50 min. Formic acid was reduced from 75% to 50%, 50- 60 min; it was reduced from 50% to 40%, 60- 65 min; it was raised from 40% to 75%, 65 - 70 min; and it was maintained at 75%. The flow rate was 1.0 mL/min, detection wavelength was 280 nm, the column temperature was 20℃, and sample size was 5 μL. RESULT Pinostrobin in the sample can reach the baseline separation with the interference groups. With this determination method the linear range of pinostrobin was 0. 101 - 0.707 μg, repetitive experiment RSD = 1.27 % （ n = 5）, average recovery rate was 98.2 % （ n = 5）, RSD = 1.89 %, and the content of pinostrobin in the sample was 16 %. CONCLUSION This method has the advantage of easy preparation of solution, with good repeatability.
出处
《南京中医药大学学报》
CAS
CSCD
2008年第3期171-172,共2页
Journal of Nanjing University of Traditional Chinese Medicine
基金
教育部“春晖”计划(Z2006-1-81003)
青海省科技厅项目(2007-N-534)-(中国药典)2010版一部标准研究(YS-130)
关键词
镰形棘豆
球松素
含量测定
反相高效液相色谱法
falcate crazyweed
pinostrobin
content determination
reversed phase high-performance liquid chromatography
