红花注射液黄酮醇类成分含量测定及特征图谱研究  

Determination and specific chromatogram study of flavonols in saffron injection for the quality control by HPLC

作　　者：窦春艳[1] 秦雪梅[1] 董红红[1] 张军[1] 郭小青[1] 张丽增[1] 

机构地区：[1]山西大学中医药现代研究中心,山西太原030006

出　　处：《中国医院药学杂志》2009年第21期1846-1849,共4页Chinese Journal of Hospital Pharmacy

摘　　要：目的:建立红花注射液中黄酮醇类成分的含量测定及特征图谱研究方法,对样品中3个指标成分羟基红花黄色素A、山柰素和槲皮素的含量进行加速实验以考察其稳定性。为控制红花注射液的质量提供参考。方法:高效液相色谱法同时测定红花注射液中山柰素及槲皮素的含量,色谱条件为色谱柱ODS-BP(200mm×4.6mm,5μm);流动相为乙腈-0.05%磷酸(28∶72);检测波长360nm;特征图谱色谱条件为色谱柱ODS-BP(200mm×4.6mm,5μm);流动相为乙腈-0.05%磷酸,梯度洗脱;检测波长345nm;加速实验条件为(40±2)℃,相对湿度(75±5)%,每月取样一次考察。结果:含量测定中槲皮素在3.6～43.68μg之间线性关系良好,Y=2E+6X-22.3(E+3)(r=0.9995),山柰素在32.4～270μg之间线性关系良好Y=3E+6X-7.61(E+3)(r=0.9999),2个组分在注射液及药材中的平均回收率在97.33%～103.1%之间,且精密度、稳定性、重复性皆满足含量测定要求。注射液特征图谱分析方法具有较好的重复性、精密度和稳定性,得到13个共有峰。加速实验可得山柰素较稳定,槲皮素次之。结论:建立了较完善的红花注射液质量控制方法,其含量测定方法专属性强、准确、稳定;特征图谱分析方法简便、快速,可全面评价红花注射液的质量。OBJECTIVE To establish a method for determination and specific chromatogram of saffron injection for the quality control. Accelerated test was used to study the stability of three index components in saffron injection sample. METHODS Conditions for determination： column ODS-BP （200 mm × 4. 6mm, 5 μm） ; mobile phase： acetonitrile-0. 05% phosphoric acid （28：72） ; wavelength：360 nm; conditions for fingerprint：Column ODS-BP （200 mm×4. 6 mm,5 μm） ; The mobile phase was a linear gradient from 15% （v/v） acetonitrile to 30% ; wavelength： 345 nm; Accelerated test conditions： 40 ± 2℃, relative humidity 75 % ± 5 %. RESULTS Quercetin had good linear relationship between 3. 6μg and 43. 68μg,y = 2E ＋ 6x - 22. 3E ＋ 3 （r = 0. 999 5） ,kaempferol had good linear relationship between 32. 4 μg and 270/xg,y= 3E＋ 6x - 7. 61 E＋ 3 （r= 0. 999 9） ,preci sion and repeatability were good, stability was good in 24 h. The average recovery rate of two components in drug and injection was between 97. 33% and 103. 1%. Studies show that chromatographic fingerprint with better reproducibility, precision and sta bility, have a total of 13 peaks. The result of accelerated test indicates that kaempferol is more stable. CONCLUSION This work has established a perfect method for quality control of safflower injection. The determination method is specific,accurate, stable and specific chromatogram can be used for comprehensive evaluation of the quality of saffron injection.

关 键 词：高效液相色谱法 红花注射液 红花药材 槲皮素 山柰素 特征图谱 

分 类 号：R927.2[医药卫生—药学]