HPLC法同时测定续断药材中7个成分的含量
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篇名: HPLC法同时测定续断药材中7个成分的含量
TITLE: Simultaneous determination of 7 components in Dipsacus asper by HPLC
摘要: 目的 建立同时测定续断药材中6个环烯醚萜类成分(马钱苷酸、马钱子苷、当药苷、续断苷B、续断苷A、林生续断苷Ⅰ)和1个三萜皂苷类成分(川续断皂苷Ⅵ)含量的方法。方法采用高效液相色谱(HPLC)法。以Symmetry®C18为色谱柱,以乙腈-0.1%磷酸溶液为流动相进行梯度洗脱,检测波长为212nm(川续断皂苷Ⅵ)、237nm(续断苷B、续断苷A、当药苷、马钱苷酸、林生续断苷Ⅰ、马钱子苷),柱温为30℃,流速为1.0mL/min,进样量为20μL。结果马钱苷酸、马钱子苷、当药苷、林生续断苷Ⅰ、续断苷B、续断苷A、川续断皂苷Ⅵ检测质量浓度的线性范围分别为399.24~931.56、50.30~150.90、48.24~168.84、27.00~70.20、12.93~38.80、40.64~121.92、42.08~147.28µg/mL(r均大于0.9990);精密度、重复性、稳定性(24h)试验的RSD均小于2%;平均加样回收率分别为104.43%(RSD=0.63%,n=6)、101.74%(RSD=1.11%,n=6)、100.76%(RSD=1.06%,n=6)、98.00%(RSD=1.58%,n=6)、99.03%(RSD=2.31%,n=6)、102.93%(RSD=2.26%,n=6)、102.31%(RSD=1.00%,n=6);含量分别为142.5~280.6、5.5~49.0、28.0~112.9、7.2~35.8、4.4~16.9、17.2~79.3、0.8~54.5mg/g。结论所建含量测定方法准确、可靠,可用于续断药材中7个成分的含量测定。
ABSTRACT: OBJECTIVE To establis h the method for the simultaneous determination of six iridoids (loganic acid ,loganin, sweroside,dipsanoside B ,dipsanoside A ,sylvestroside Ⅰ)and one triterpene saponin (asperosaponin Ⅵ)in Dipsacus asper . METHODS High performance liquid chromatography (HPLC) method was adopted. The determination was performed on Symmetry® C18 column with mobile phase consisted of acetonitrile- 0.1% phosphoric acid solution (gradient elution )at the flow rate of 1.0 mL/min. The detection wavelengths were set at 212 nm(asperosaponin Ⅵ)and 237 nm(dipsanoside B ,dipsanoside A , sweroside,loganic acid ,sylvestroside Ⅰ,loganin). The column temperature was set at 30 ℃,and sample size was 20 μL. RESULTS The linear range of loganic acid , loganin, sweroside, sylvestroside Ⅰ , dipsanoside B , dipsanoside A and asperosaponin Ⅵ were 399.24-931.56,50.30-150.90,48.24-168.84,27.00-70.20,12.93-38.80,40.64-121.92,42.08-147.28 µg/mL (all r>0.999 0). RSDs of precision ,reproducibility and stability tests (24 h)were all less than 2%. Average recoveries were 104.43%(RSD=0.63%,n=6),101.74%(RSD=1.11%,n=6),100.76%(RSD=1.06%,n=6),98.00%(RSD=1.58%,n=6), 99.03%(RSD=2.31%,n=6),102.93%(RSD=2.26%,n=6),102.31%(RSD=1.00%,n=6),respectively,The contents were 142.5-280.6,5.5-49.0,28.0-112.9,7.2-35.8,4.4-16.9,17.2-79.3,0.8-54.5 mg/g,respectively. CONCLUSIONS Established method is accurate and reliable ,and can be used for the content determination of 7 components in D. asper .
期刊: 2022年第33卷第06期
作者: 杨昌贵,龚安慧,张成刚,肖承鸿,凡迪,周涛
AUTHORS: YANG Changgui,GONG Anhui,ZHANG Chenggang,XIAO Chenghong,FAN Di,ZHOU Tao
关键字: 续断;含量测定;高效液相色谱法;三萜皂苷;环烯醚萜
KEYWORDS: Dipsacus asper ;content determination ;high performance liquid chromatography ;triterpene saponins ;iridoids
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