摘要
目的：建立梯度洗脱法同时测定阿胶益寿晶中二苯乙烯苷、大黄素甲醚、毛蕊异黄酮苷、芒柄花苷、毛蕊异黄酮和芒柄花素含量的高效液相色谱法。方法：采用Agilent TC-C18色谱柱（4.6 mm×250 mm,5μm）,流动相A乙腈-甲醇（9∶1）,流动相B 0.1%磷酸溶液梯度洗脱,柱温30℃,流速1.0 m L·min-1,进样量20μL;二苯乙烯苷和大黄素甲醚检测波长为280nm,毛蕊异黄酮苷、芒柄花苷、毛蕊异黄酮和芒柄花素检测波长为254 nm。结果：二苯乙烯苷、大黄素甲醚、毛蕊异黄酮苷、芒柄花苷、毛蕊异黄酮和芒柄花素分别在5.23-104.60 mg·L-1（r=0.999 5）,5.05-101.00 mg·L-1（r=0.999 1）,5.92-118.40 mg·L-1（r=0.999 3）,4.74-94.80 mg·L-1（r=0.999 8）,4.85-97.00 mg·L-1（r=0.999 7）,6.91-138.20 mg·L-1（r=0.999 7）线性关系良好;平均加样回收率（n=6）和RSD分别为98.52%（1.6%）,97.95%（1.4%）,99.47%（1.6%）,96.99%（1.0%）,99.24%（1.1%）,98.13%（1.4%）。结论：建立的HPLC梯度洗脱法同时测定阿胶益寿晶中二苯乙烯苷、大黄素甲醚、毛蕊异黄酮苷、芒柄花苷、毛蕊异黄酮和芒柄花素含量。方法准确、灵敏度高、重复性好,为评价阿胶益寿晶质量控制提供可靠方法。
Objective： To establish an HPLC gradient elution method for simultaneous determination of stibene glucoside,physcione,calycosin-7-O-β-D-glucoside,ononin,calycosin and fermlononetin in Ejiao Yishou Jing. Method： An Agilent TC-C18column（ 4. 6 mm × 250 mm,5 μm）,with acetonitrile-methanol（ 9 ∶1）（ A）and 0. 1% phosphate acid solution（ B） as the mobile phases for gradient elution. The column temperature was 30℃,and the flow rate was 1. 0 m L·min-1,with an injection volume of 20 μL. Stibene glucoside and physcione were detected at 280 nm; calycosin-7-O-β-D-glucoside,ononin,calycosin and fermlononetin were detected at 254 nm. Result： Stibene glucoside,physcione,calycosin-7-O-β-D-glucoside,ononin,calycosin and fermlononetin showed good linearity within the concentration range of 5. 23-104. 60 mg·L-1（ r = 0. 999 5）,5. 05-101. 00mg·L-1（ r = 0. 999 1）,5. 92-118. 40 mg·L-1（ r = 0. 999 3）,4. 74-94. 80 mg·L-1（ r = 0. 999 8）,4. 85-97. 00mg·L-1（ r = 0. 999 7）,and 6. 91-138. 20 mg·L-1（ r = 0. 999 7） respectively. Their average recovery rate（ n =6） and RSD were 98. 52%（ 1. 6%）,97. 95%（ 1. 4%）,99. 47%（ 1. 6%）,96. 99%（ 1. 0%）,99. 24%（ 1. 1%）,and 98. 13%（ 1. 4%） respectively. Conclusion： This HPLC gradient elution method could be used to simultaneously determine the contents of stibene glucoside,physcione, calycosin-7-O-β-D-glucoside, ononin,calycosin and fermlononetin in Ejiao Yishou Jing. This method is accurate,highly sensitive and repeatable,providing a reliable method for the quality control of Ejiao Yishou Jing.
出处
《中国实验方剂学杂志》
CAS
CSCD
北大核心
2016年第23期68-72,共5页
Chinese Journal of Experimental Traditional Medical Formulae
基金
吉林省科技发展计划项目(20140311029YY)
关键词
阿胶益寿晶
二苯乙烯苷
大黄素甲醚
毛蕊异黄酮苷
芒柄花苷
毛蕊异黄酮
芒柄花素
HPLC
gradient elution method
Ejiao Yishou Jing
stibene glucoside
physcione
calycosin-7-O-β-D-glucoside
ononin
calycosin
fermlononetin
