摘要
采用高效液相色谱法测定四季三黄丸中栀子苷、盐酸小檗碱、黄芩苷和大黄素的含量。样品经甲醇超声提取后,利用Phenomenex Luna C_(18)色谱柱进行分离,以乙腈-0.1%(体积分数)甲酸溶液为流动相进行梯度洗脱,采用二极管阵列检测器,栀子苷、盐酸小檗碱、黄芩苷和大黄素检测波长分别为240,345,278,287nm。栀子苷、盐酸小檗碱、黄芩苷和大黄素的线性范围分别为7.66~76.6,8.99~89.9,3.87~38.7,4.45~44.5mg·L^(-1),检出限(3S/N)分别为0.27,0.038,0.037,0.048mg·L^(-1)。加标回收率在96.3%~99.5%之间,测定值的相对标准偏差(n=6)在1.7%~2.4%之间。
HPLC was applied to the determination of geniposide, berberine hydrochloride, baicalin and emodin in Siji Sanhuang pills. The sample was extracted ultrasonically with methanol. The extract was separated on a Phenomenex Luna C18 column with gradient elution using acetonitrile and 0. 1 % (φ) formic acid solution as mobile phase. Diode array detector was used with the detection wavelengths of 240, 345, 278, 287 nm, for geniposide, berberine hydrochloride, baiealin and emodin, respectively. Linearity ranges of geniposide, berberine hydrochloride, baicalin and emodin were 7. 66--76. 6, 8. 99--89. 9, 3. 87--38. 7, 4. 45--44. 5 mg · L-1, respectively'. The detection limits (3S/N) were 0. 27, 0. 038, 0. 037, 0. 048 mg· L 1, respectively. Recovery rates obtained by standard additon method ranged from 96.3% to 99.5%, and RSDs (n=6) were in the range of 1.7%-2.4%.
出处
《理化检验(化学分册)》
CSCD
北大核心
2017年第6期669-673,共5页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
上海市技术性贸易措施应对专项项目(14TBT007
15TBT009)