高效液相色谱法同时测定丹膝颗粒中8种成分的含量

Simultaneous Determination of Eight Components in Dan Xi Granules by HPLC

目的建立高效液相色谱(HPLC)法同时测定丹膝颗粒中天麻素、栀子苷、丹酚酸B、淫羊藿苷、橙黄决明素、丹参酮Ⅰ、隐丹参酮和丹参酮ⅡA的含量。方法以70%甲醇提取供试样品;采用Agilent ZORBAX SB-C18色谱柱(250 mm×4.6 mm,5μm);流动相为乙腈-0.2%磷酸水溶液,梯度洗脱;流速:1.0 mL·min-1;柱温:30℃,检测波长为220、238、280 nm。结果天麻素、栀子苷、丹酚酸B、淫羊藿苷、橙黄决明素、丹参酮Ⅰ、隐丹参酮和丹参酮ⅡA质量浓度分别在2.105~21.05μg·mL-1(r=0.9994)、10.54~105.4μg·mL-1(r=0.9993)、23.52~235.2μg·mL-1(r=0.9998)、3.409~34.09μg·mL-1(r=0.9997)、0.6834~6.834μg·mL-1(r=0.9999)、1.013~10.13μg·mL-1(r=0.9997)、1.394~13.94μg·mL-1(r=0.9998)和1.491~14.91μg·mL-1(r=0.9998)范围内与峰面积呈良好的线性关系;平均回收率(n=6)分别为98.56%(RSD=2.74%)、98.99%(RSD=1.16%)、100.34%(RSD=2.09%)、97.86%(RSD=1.41%)、94.66%(RSD=2.05%)、99.49%(RSD=2.61%)、95.89%(RSD=1.24%)和101.07%(RSD=2.97%)。结论该方法准确度高、重复性好,可为丹膝颗粒的质量控制提供参考。

Objective To establish an HPLC method for simultaneous determination of gastrodin,gemposide,salvianolic acid B,icariin,aurantio-obtusin,tanshinoneⅠ,cryptotanshinone and tanshinoneⅡA in Dan Xi granules.Methods The analysis of 70%methanol extract of this drug was performed on Agilent ZORBAX SB-C18column(250 mm×4.6 mm,5μm)by gradient elution with acetonitrile-0.2%phosphoric acid solution at a flow rate of 1.0 mL·min-1.The column temperature was 30℃and the detection wavelength was set at 220 nm,238 nm,280 nm.Results Good linear relationships were fund for gastrodin,geniposide,salvianolic acid B,icariin,aurantio-obtusin,tanshinoneⅠ,cryptotanshinone and tanshinoneⅡA in the ranges of 2.105-21.05μg·mL-1(r=0.9994),10.54-105.4μg·mL-1(r=0.9993),23.52-235.2μg·mL-1(r=0.9998),3.409-34.09μg·mL-1(r=0.9997),0.6834-6.834μg·mL-1(r=0.9999),1.013-10.13μg·mL-1(r=0.9997),1.394-13.94μg·mL-1(r=0.9998)and 1.491-14.91μg·mL-1(r=0.9998),respectively.The average recoveries(n=6)were 98.56%(RSD=2.74%),98.99%(RSD=1.16%),100.34%(RSD=2.09%),97.86%(RSD=1.41%),94.66%(RSD=2.05%),99.49%(RSD=2.61%),95.89%(RSD=1.24%)and 101.07%(RSD=2.97%),respectively.Conclusion The method is accurate and reproducible,and can provide reference for the quality control of Dan Xi granules.