HPLC波长切换法同时测定琥珀多寐丸中6个成分的含量

Simultaneous determination of 6 components in hupoduomei pill by HPLC method with UV wavelengths switch

目的建立同时测定琥珀多寐丸中远志(口山)酮Ⅲ、3,6'-二芥子酰基蔗糖、细叶远志皂苷、远志皂苷B、去氢土莫酸和茯苓酸含量的方法。方法采用波长切换检测的高效液相色谱法,色谱柱采用依利特C_(18)色谱柱,流动相为乙腈(A)-体积分数为0.1%的磷酸溶液(B)系统,进行梯度洗脱;0~36 min检测波长为320 nm(检测远志(口山)酮Ⅲ、3,6'-二芥子酰基蔗糖),36~75 min检测波长为210 nm(检测细叶远志皂苷、远志皂苷B、去氢土莫酸、茯苓酸);流速为1.3 mL·min^(-1);柱温为30℃。结果在优化的色谱条件下,远志(口山)酮Ⅲ、3,6'-二芥子酰基蔗糖、细叶远志皂苷、远志皂苷B、去氢土莫酸和茯苓酸分别在6.46~129.20 mg·L^(-1)(r=0.999 2)、6.13~122.60 mg·L^(-1)(r=0.999 5)、13.17~263.40 mg·L^(-1)(r=0.999 9)、14.15~283.00 mg·L^(-1)(r=0.999 6)、5.35~107.00 mg·L^(-1)(r=0.999 7)、4.50~90.00 mg·L^(-1)(r=0.999 3)内浓度与峰面积呈良好的线性关系;6种成分的平均加样回收率(n=6)分别为97.69%、96.87%、100.04%、97.74%、97.67%、99.16%,RSD分别为1.35%、0.96%、0.59%、0.93%、1.02%、1.10%。结论该检测方法可用于琥珀多寐丸中远志(口山)酮Ⅲ、3,6'-二芥子酰基蔗糖、细叶远志皂苷、远志皂苷B、去氢土莫酸和茯苓酸的含量分析。

Objective To establish a method for the simultaneous determination of six main components including polygalaxanthone Ⅲ,3,6＇-disinapoyl sucrose, tenuifolin,onjisaponin B,dehydrotumulosic acid and pachymic acid in hupoduomei pill.Methods A HPLC method with UV wavelength switch had been developed and detection wavelength was set at 320 nm within the period of 0-36 min for polygalaxanthone Ⅲ,3,6＇-disinapoyl sucrose,and then switched to 210 nm within 36-75 min for tenuifolin,onjisaponin B,dehydrotumulosic acid,and pachymic acid. The separation was performed on a Hypersil C_（18） column and a mixture of acetonitrile and 0. 1% phosphate acid was adopted as the mobile phase. The flow rate was 1. 3 mL·min^（-1）. The column temperature was at 30 ℃. Results The linear response range was 6. 46-129. 20 mg·L^（-1）（ r = 0. 999 2） for polygalaxanthone Ⅲ,6. 13-122. 60 mg·L^（-1）（ r = 0. 999 5） for 3,6＇-disinapoyl Sucrose,13. 17-263. 40 mg·L^（-1）（ r = 0. 999 9） for tenuifolin,14. 15-283. 00 mg·L^（-1）（ r =0. 999 6） for onjisaponin B,5. 35-107. 00 mg·L^（-1）（ r = 0. 999 7） for dehydrotumulosic acid and 4. 50-90. 00 mg·L^（-1）（ r = 0. 999 3） for pachymic acid. The average recoveries and RSD were 97. 69%（ 1. 35%）,96. 87%（ 0. 96%）,100. 04%（ 0. 59%）,97. 74%（ 0. 93%）,97. 67%（ 1. 02%） and 99. 16%（ 1. 10%）,respectively. Conclusions The method is economic,accurate and highly specific with good reproducibility.