HPLC-波长切换法同时测定消栓肠溶胶囊中7个成分的含量

目的:建立同时测定消栓肠溶胶囊中7个活性成分绿原酸、苦杏仁苷、芍药苷、阿魏酸、洋川芎内酯Ⅰ、毛蕊异黄酮苷和藁本内酯的含量。方法:采用高效液相色谱法,色谱柱为Agilent Eclipse Plus C18,流动相为乙腈-0.1%磷酸溶液,梯度洗脱,检测波长为326 nm(绿原酸)、210 nm(苦杏仁苷)、230 nm(芍药苷)、321 nm(阿魏酸)、334(洋川芎内酯Ⅰ)、274 nm(毛蕊异黄酮苷)、260 nm(藁本内酯),流速为1.0 mL/min,柱温为35℃,进样量为10μL。结果:绿原酸、苦杏仁苷、芍药苷、阿魏酸、洋川芎内酯Ⅰ、毛蕊异黄酮苷和藁本内酯检测质量浓度的线性范围分别为1.16~34.81、1.85~55.48、13.22~396.50、13.50~405.09、1.75~52.51、2.74~82.18、7.67~230.07μg/mL(r为0.999 1~0.999 7);定量限分别为0.056、0.103、0.085、0.013、0.136、0.184、0.276μg;精密度、稳定性(24 h)、重复性试验的RSD<2.0%(n=6);平均回收率分别为99.3%、98.6%、98.8%、99.7%、97.1%、97.6%和99.2%(RSD<2.0%,n=6)。结论:建立的含量测定方法操作简便、结果准确,可用于消栓肠溶胶囊中7个成分的同时测定。

Simultaneous Determination of 7 Constituents in Xiaoshuan Enteric-coated Capsules by HPLC-wavelength Switching Method

OBJECTIVE:To establish a method for simultaneous determination of 7 active constituents in Xiaoshuan entericcoated capsules,such as chlorogenic acid,amygdalin,paeoniflorin,ferulic acid,senkyunolide Ⅰ,calycosin glycoside and ligustilide. METHODS:HPLC method was adopted. The determination was performed on Agilent Eclipse Plus C18 column with mobile phase consisted of acetonitrile-0.1% phosphoric acid(gradient elution). The detection wavelengths were set at 326 nm for chlorogenic acid,210 nm for amygdalin,230 nm for paeoniflorin,321 nm for ferulic acid,334 nm for senkyunolideⅠ,274 nm for calycosin glycoside and 260 nm for ligustilide. The flow rate was set at 1.0 mL/min,and the column temperature was 35 ℃.The sample size was 10 μL. RESULTS:The linear range was 1.16-34.81 μg/mL for chlorogenic acid,1.85-55.48 μg/mL for amygdalin,13.22-396.50 μg/mL for paeoniflorin,13.50-405.09 μg/mL for ferulic acid,1.75-52.51 μg/mL for senkyunolideⅠ,2.74-82.18 μg/mL for calycosin glycoside,7.67-230.07 μg/mL for ligustilide(r=0.999 1-0.999 7),respectively. The limit of quantity were 0.056,0.103,0.085,0.013,0.136,0.184 and 0.276 μg. RSDs of precision,stability(24 h) and reproducibility tests were lower than 2.0%(n=6). Average recoveries were 99.3%,98.6%,98.8%,99.7%,97.1%,97.6% and 99.2%(RSD<2.0%,n=6). CONCLUSIONS:Established method is accurate and simple. It can be used for simultaneous determination of 7 constituents in Xiaoshuan enteric-coated capsules.