RP-HPLC波长切换法同时测定治偏痛颗粒中原儿茶酸等5种成分的含量

Simultaneous determination of five constituents content in Zhipiantong granules by RP-HPLC wavelength switching method

目的建立RP-HPLC波长切换法同时测定治偏痛颗粒中原儿茶酸、芍药内酯苷、芍药苷、阿魏酸和藁本内酯共5种成分的含量。方法以Platisil ODS（250 mm×4.6 mm,5μm）为色谱柱,乙腈-体积分数为0.1%的磷酸溶液为流动相进行梯度洗脱,流速为1.0 m L·min^-1,柱温为35℃,检测波长为0～30 min时为230 nm和30～65 min时为320 nm,进样量为20μL。结果原儿茶酸、芍药内酯苷、芍药苷、阿魏酸和藁本内酯的质量浓度分别在5.05～50.5 mg·L^-1（r=0.999 3,n=6）、11.30～113.0 mg·L^-1（r=0.999 3,n=6）、24.08～240.8 mg·L^-1（r=0.999 9,n=6）、1.40～14.0 mg·L^-1（r=1.000,n=6）和1.76～17.6 mg·L^-1（r=1.000,n=6）内与峰面积呈良好的线性关系,方法的平均回收率分别为98.3%（RSD=0.5%,n=9）、98.9%（RSD=0.4%,n=9）、99.7%（RSD=0.4%,n=9）、101.8%（RSD=0.8%,n=9）和102.3%（RSD=1.4%,n=9）。结论所建立的高效液相色谱测定法可用于治偏痛颗粒的质量控制。

Objective To develop an RP-HPLC wavelength switching method for determination of protocate- chuic ,albiflorin,paeom＇florin,ferulic acid and ligusutilde in Zhipiantong granules. Methods The HPLC separa- tion was achieved on a Platisil ODS（250 mm ×4. 6 mm,5 μm）column at 35 ℃. The mobile phase consisted of acetonirile -0. 1% phosphoric acid solution with gradient elution at a flow rate of 1.0 mL· min^-1. The UV detection wavelength was set at 230 nm,in 0- 30 min; at 320 nm,in 30- 65 min. Results The linear ranges were 5.05-50. 5 mg·L^-1 （r =0. 999 3 ,n =6） ,11.30- 113.0 mg·L^-1 （ r =0. 999 3 ,n =6） ,24. 08- 240. 8 mg·L^-1 （ r =0. 999 9,n =6）, 1.40- 14. 0 mg·L^-1 （r = 1. 000,n =6）and 1.76- 17. 6 mg·L^-1（r = 1. 000,n =6） ,respec- tively. The recoveries were 98. 3% （ RSD = 0. 5%, n = 9 ）, 98.9% （ RSD = 0. 4%, n = 9 ）, 99. 7% （ RSD = 0. 4%, n = 9）, 101.8 % （RSD = 0. 8 %, n = 9 ）and 102. 3 % （RSD = 1.4%, n = 9）, respectively. Conclusions The method is simple, accurate and repeatable and can be used for quality control of Zhipiantong granules.