摘要
目的:建立UPLC同时测定秦皮配方颗粒中7种成分(秦皮甲素、毛柳苷、秦皮乙素、丁香苷、秦皮苷、秦皮素和东莨菪内酯)的方法,比较不同厂家及批次秦皮配方颗粒中7种成分含量的差异,为秦皮配方颗粒的科学质量控制提供依据。方法:采用Waters超高效液相色谱仪,Waters ACQUITY UPLC BEH C_(18)色谱柱(2.1 mm×50 mm,1.7μm),以甲醇(A)-0.1%磷酸水溶液(B)为流动相,梯度洗脱(0~1 min,5%~10%A;1~10 min,10%~12%A),流速0.4 m L·min^(-1),进样量2μL,柱温38℃,检测波长220 nm。结果:色谱峰纯度结果表明方法专属性良好。秦皮甲素、毛柳苷、秦皮乙素、丁香苷、秦皮苷、秦皮素和东莨菪内酯分别在各自范围内峰面积与浓度呈良好的线性关系;平均回收率分别为100.0%(RSD 2.0%),99.5%(RSD2.1%),99.9%(RSD 1.5%),99.7%(RSD 2.2%),99.4%(RSD 1.4%),100.8%(RSD 1.8%),99.4%(RSD 2.6%)。结论:该方法简便、准确,适用于秦皮配方颗粒中7种成分的同时定量测定,分析时间明显缩短,并对秦皮配方颗粒中除秦皮甲素和秦皮乙素之外的多种成分首次进行了定量测定,不同厂家及批次的秦皮配方颗粒主要成分含量存在一定的差异。
Objective： To establish a UPLC method for the simultaneous determination of aesculin, salidroside, aesculetin, syringin, fraxin, fraxetin and scopoletin in the Fraxini Cortex formula granule, in order to compare the difference of the seven chemical constituents in various Fraxini Cortex formula granule samples and provide an effective method to ensure the scientific quality of Fraxini Cortex formula granule. Method： The separation was performed on a Waters ACQUITY UPLC BEH C1s column （2. 1 mm ×50 mm, 1.7μm） , and eluted with mobile phase consisting of methanol-0.1% phosphoric acid solution in a gradient mode （0-1 min, 5%-10% A; 1-10 min, 10% -12% A） at a flow rate of 0.4 mL.min-1. The sample size was 2 μL. The detection wavelength was 220 nm, and the column temperature was 38℃. Result： Peak area and concentration for aesculin, salidroside, aeseuletin, syringing, fraxin, fraxetin and seopoletin showed a good linearity within their ranges, the average recoveries of the chemical constituents were 100.0% （ RSD 2.0% ）, 99.5% （ RSD 2. 1% ）, 99.9% （RSD 1.5%）,99.7% （RSD2.2%）,99.4% （RSD 1.4%）, 100.8% （RSD1.8%）,99.4% （RSD2.6%）, respectively. Conclusion： The established method is simple and accurate, and can be used to simultaneously determine seven chemical constituents in Fraxini Cortex formula granule, and the analysis time was significantly shortened. It＇s the first time to make a quantitative determination for many ingredients except for aesculin and the aesculetin in the Fraxini Cortex formula granule. There are certain differences in the contents of chemical compositions in the Fraxini Cortex formula granule of various batches and manufacturers.
出处
《中国实验方剂学杂志》
CAS
CSCD
北大核心
2017年第11期63-67,共5页
Chinese Journal of Experimental Traditional Medical Formulae
基金
国家自然科学基金项目(81102412)
