HPLC-ELSD测定舒血宁注射液的化学成分及含量  

Separate and Determine the Chemical Composition of Shuxuening Injection by HPLC-ELSD

作　　者：冯子明 苑祥 杨桠楠 姜建双 张旭 张培成 FENG Ziming;YUAN Xiang;YANG Ya'nan;JIANG Jianshuang;ZHANG Xu;ZHANG Peicheng(Institute of Materia Medica,Chinese Academy of Medical Sciences and Peking Union Medical College/'State Key Laboratory of Active Substances and Functions of Natural Medicines,Bejing China 100050)

机构地区：[1]中国医学科学院北京协和医学院药物研究所/天然药物活性物质与功能国家重点实验室,北京100050

出　　处：《中医学报》2020年第6期1266-1270,共5页Acta Chinese Medicine

摘　　要：目的:通过高效液相色谱-蒸发光散射检测器(high performance liquid chromatography-evaporative light scattering detector,HPLC-ELSD)分离发现舒血宁注射液中的不含紫外吸收的化学成分并测定含量。方法:直接通过HPLC-ELSD导向分离,富集相应色谱峰的组分,通过1D和2D NMR,MS,并参照对照品确定了舒血宁注射液中的化学成分。采用HPLC-ELSD方法同时测定分离得到的成分含量,条件为:色谱柱:COSMOSIL5NH2-MS氨基柱(5μm,4.6 mm×250.0 mm),流速:1.0 mL·min^-1,柱温:30℃,漂移管温度60℃,增益4,流动相为:乙腈水(89∶11)。结果:分离鉴定了舒血宁注射液中的4个化学成分,分别为松醇、果糖、红杉醇、葡萄糖,其中松醇和红杉醇为首次发现。含量测定方面,以峰面积的自然对数对质量的自然对数进行线性回归,松醇质量在4.4232~22.1160μg范围内与峰面积对数呈良好线性关系,r=0.9999(n=6),平均回收率为101.34%(n=9);果糖质量在6.1223~30.6113μg范围内与峰面积对数呈良好线性关系,r=1.0000(n=6),平均回收率为102.19%(n=9);红杉醇质量在1.7875~8.9376μg范围内与峰面积对数呈良好线性关系,r=0.9989(n=6),平均回收率为101.12%(n=9);葡萄糖质量在7.7583~38.7917μg范围内与峰面积对数呈良好线性关系,r=0.9948(n=6),平均回收率为101.02%(n=9)。结论:完善了舒血宁注射液化学质量控制方法,该含量测定方法简便、快速,结果准确、可靠、重复性良好,可用于舒血宁注射液中松醇、果糖、红杉醇和葡萄糖的含量测定。Objective:To isolate and detect the chemical components in Shuxuening Injection without ultraviolet absorption by high performance liquid chromatography-evaporative light scattering detector(HPLC-ELSD).Method:Directly separate by HPLCELSD,enrich the components of corresponding chromatographic peaks,and determine the chemical composition of Shuxuening Injection by 1D and 2D NMR,MS,and control method.HPLC-ELSD method was used to simultaneously determine the content of the separated components under the following conditions:chromatography column:COSMOSIL5NH2-MS amino column(5μm,4.6 mm×250 mm),flow rate:1.0 mL·min^-1,column temperature:30℃,The drift tube temperature is 60℃,the gain is 4,and the mobile phase is acetonitrile water(89:11).Results:Four chemical components in Shuxuening injection were isolated and identified,namely pinitol,fructose,taxol,and glucose,among which pinitol and taxol were first discovered;in terms of content determination,the natural The logarithm of the natural logarithm of the logarithmic mass is linearly regressed.The mass of pinitol in the range of 4.4232-22.1160μg has a good linear relationship with the logarithm of the peak area.;The fructose quality is in a linear relationship with the logarithm of the peak area in the range of 6.1223-30.6113μg,r=1.0000(n=6),the average recovery rate is 102.19%(n=9);the mass of taxol is 1.7875-8.9376 There is a good linear relationship with the logarithm of the peak area in the range ofμg,r=0.9989(n=6),the average recovery rate is 101.12%(n=9);the mass of glucose is in the range of 7.7583-38.7917μg and the logarithm of the area Linear relationship,r=0.9948(n=6),the average recovery rate is 101.02%(n=9).Conclusion:The chemical quality control method of Shuxuening Injection has been improved.The content determination method is simple,fast,and the results are accurate and reliable,with good repeatability.It can be used for Zhongsong Determination of alcohol,fructose,taxol and glucose in Shuxuening Injection.

关 键 词：舒血宁注射液 高效液相色谱-蒸发光散射检测器法 松醇 红杉醇 果糖 葡萄糖 银杏叶 

分 类 号：R284.2[医药卫生—中药学]