高效液相色谱法对大川芎片中5种成分的含量测定

目的 本研究通过运用高效液相色谱法建立大川芎片的特征图谱,并对洋川芎内酯Ⅰ、绿原酸、洋川芎内酯A、香草酸、阿魏酸5种指标性成分进行含量测定.方法 本试验采用Agilent Poroshell SB-C18色谱柱(4.6 mm×100 mm,2.7 μm),流动相0.02%甲酸水(A)-乙腈(B)溶液梯度洗脱,检测波长280 nm,流速0.8 mL·min-1,柱温30 ℃,记录时间40 min,对同一厂家10批次大川芎片进行含量测定.结果 本试验初步建立了大川芎片的高效液相特征色谱图,指标性成分洋川芎内酯Ⅰ、绿原酸、洋川芎内酯A、香草酸、阿魏酸均达到基线分离,其线性范围分别为3~48 nL(r=0.999 9),0.062 2~0.995 5 μg(r=0.999 8),0.3~4.8 nL(r=0.999 9),0.026 6~0.426 2 μg(r=0.999 9),0.016 9~0.270 7 μg(r=0.999 7).加样回收率均在95%~105%之间,精密度、稳定性、重复性均良好.结论 以洋川芎内酯Ⅰ、绿原酸、洋川芎内酯A、香草酸、阿魏酸为指标性成分对大川芎片进行含量测定,该方法准确、重现性好,可以全面地反映大川芎片质量,为大川芎片质量控制奠定基础.

Determination of 5 components of Dachuanxiong Tablets by HPLC method

Objective To establish the fingerprint of Dachuanxiong Tablets by HPLC methods,and determine the 5 kinds of index components contents such as senkyunolide Ⅰ,chlorogenic acid,senkyunolide A,vanillic acid,ferulic acid.Methods Agilent poroshell SB-C18 column(4.6 mm×100 mm,2.7 μm) was adopted,the mobile phase was 0.02% formic acid water(A)-acetonitrile(B) solution with gradient elution,the detection wavelength was 280 nm, the flow rate was 0.8 mL·min-1,the column temperature was 30 ℃,and the recording time was 40 min.The contents of 10 different batches of Dachuanxiong Tablets from same manufacturer were determined.Results This study established the HPLC fingerprint of Dachuanxiong Tablets,the index component of senkyunolide Ⅰ,chlorogenic acid,senkyunolide A,vanillic acid and ferulic acid were separated,the linear range was 3~48 nL(r=0.999 9),0.062 2~0.995 5 μg(r=0.999 8),0.3~4.8 nL(r=0.999 9),0.026 6~0.426 2 μg(r=0.999 9),0.016 9~0.270 7 μg(r=0.999 7),respectively.The recoveries were ranged from 95% to 105%,and the precision,stability and repeatability were good.Conclusion This study used senkyunolide Ⅰ,chlorogenic acid,senkyunolide A,vanillic acid and ferulic acid as the index component for the determination of Dachuanxiong Tablets,the method was accurate and reproducible which can reflect the comprehensive quality of Dachuanxiong Tablets and can lay the foundation for quality control of Dachuanxiong Tablets.