双波长高效液相法同时测定双香排石颗粒中的马钱子苷、当药苷、断氧化马钱子苷、迷迭香酸和木通苯乙醇苷B

Simultaneous determination of loganin,chiratin,secoxyloganin,rosmarinic acid and calceolarioside B in Shuangxiangpaishi granules by dual-wavelength HPLC method

目的建立高效液相双波长切换法同时测定双香排石颗粒中马钱子苷、当药苷、断氧化马钱子苷、迷迭香酸和木通苯乙醇苷B的含量。方法采用Alltima C18色谱柱（4.6 mm×250 mm,5μm）;以乙腈-甲醇（1∶3）（A）-0.1%磷酸溶液（B）为流动相进行梯度洗脱;柱温为35℃;流速为1.0 ml/min;进样量为20μl;马钱子苷、断氧化马钱子苷和当药苷检测波长为240 nm,迷迭香酸和木通苯乙醇苷B检测波长为330 nm。结果马钱子苷、当药苷、断氧化马钱子苷、迷迭香酸和木通苯乙醇苷B在给定浓度范围内线性范围分别为5.91~118.20μg/ml（r=0.9995）、4.10~82.00μg/ml（r=0.9991）、8.13~162.60μg/ml（r=0.9993）、12.57~251.40μg/ml（r=0.9998）和4.95~99.00μg/ml（r=0.9997）,线性关系良好;平均加样回收率（n=6）和RSD值分别为96.88%（1.31%）、99.09%（1.47%）、98.29%（1.59%）、98.82%（1.42%）和97.51%（0.86%）。结论本文建立的双波长HPLC方法同时测定双香排石颗粒中马钱子苷、当药苷、断氧化马钱子苷、迷迭香酸和木通苯乙醇苷B含量。方法灵敏度高、简便、准确、重现性好,为评价双香排石颗粒质量控制提供可靠方法。

Objective To establish an HPLC method for simultaneous determination of loganin,chiratin,secoxyloganin,rosmarinic acid and calceolarioside B in Shuangxiangpaishi granules. Method HPLC colunmn was Alltima C18column（4.6 mm×250mm,5 μm）;mobile phase consisted of acetonitrile-methanol（1∶3）（A）-0.1% phosphate acid solution（B）with gradient elution;the column temperature was 35℃;the flow rate was 1.0 ml/min;all the injection volume was 20 μl;loganin,chiratin and secoxyloganin were detected at 240 nm,rosmarinic acid and calceolarioside B were detected at 330 nm. Results The above mentioned five main ingredients had linearity in the given concentration range at 5.91-118.20 μg/ml（r=0.9995）,4.10-82.00 μg/ml（r=0.9991）,8.13-162.60μg/ml（r=0.9993）,12.57-251.40 μg/ml（r=0.9998）、4.95-99.00μg/ml（r=0.9997）,respectively. The average recoveries（n=6）and RSD were 96.88%（1.31%）,99.09%（1.47%）,98.29%（1.59%）,98.82%（1.42%）and 97.51%（0.86%）,respectively. Conclusion This dual-wavelength HPLC method could simultaneously determine the contents of the five ingredients in Shuangxiangpaishi granules and can be used to evaluate their quality. The method is simple,accurate,sensitive and repeatable. It could be used as an efficient strategy for systematic quality evaluation of Shuangxiangpaishi granules。