世界中医药

作者	单位
都姣娇1，屈相玲2，张琪1	1 北京市中西医结合医院药剂科,北京,100039 2 贵阳中医学院第二附属医院药剂科,贵阳,550003

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中文摘要:

目的:通过高效液相色谱法测定丹红注射液中有效成分丹酚酸羟基红花黄色素A(以下简称丹酚酸A)、丹酚酸B、丹参素钠、原儿茶醛、咖啡酸和迷迭香酸的含量。方法:色谱条件采用C18色谱柱(型号为Eclipse XDB),该色谱柱的长度为250 mm,色谱柱内经为46 mm,色谱柱填料颗粒直径为5 μm。进样量为10 μL,流动相采用乙腈(A相)和01%磷酸水溶液(B相)的二元体系进行梯度洗脱。高效液相应用于药物成分分析中,因为高效液相系统中的DAD检测器可在色谱分析过程中自动记录色谱峰对应组分和对应波长的光谱图,本研究采用双光束紫外可见分光光度计检测6种对照品以确定检测波长。高效液相色谱法方法严谨性考察,包括线性关系、精密度、重复性、稳定性和加样回收试验考察,基于高效液相色谱法方法具有严谨性的前提下,对丹红注射液中成分的含量进行测定。结果:1)本研究采用双光束紫外可见分光光度计检测6种对照品的紫外-可见光谱分析确定检测波长为280 nm可测定丹参素钠、原儿茶醛、丹酚酸B、丹酚酸A这4种成分;而检测波长为330 nm可测定咖啡酸、迷迭香酸这2种成分。2)线性考察结果显示回归方程、相关系数和线性范围分别是:丹酚酸A:Y=162X+769、0999 9、3362~3 36200 μg/mL;丹酚酸B:Y=8431X+1884、0999 8、221~2 21000 μg/mL;丹参素钠:Y=3740X+69608、0999 1、1178~1 17800 μg/mL;原儿茶醛:Y=20345X+2102、0999 9、101~10100 μg/mL;咖啡酸:Y=118453X+248、0999 7、005~510 μg/mL;迷迭香酸:Y=20304X+6593、0999 9、108~10800 μg/mL。3)加样回收试验结果显示丹酚酸A对照品溶液、丹酚酸B对照品溶液、丹参素钠对照品溶液、原儿茶醛对照品溶液、咖啡酸对照品溶液、迷迭香酸对照品溶液平均回收率分别为10020%、10103%、9901%、10087%、10043%、9874%,RSD分别为129%、165%、129%、1035%、132%、184%,提示高相液相检测方法所测加样回收率结果可靠。4)混合对照品溶液和丹红注射液供试品溶液的HPLC色谱图可见丹红注射液供试品溶液中6种成分与其他共存峰均得到很好的分离,3个不同批次的丹红注射液中成分含量均存在不同程度的差异。结论:高效液相色谱法的操作简单,结果具有较好的精密度、稳定性和重复性,可作为丹红注射液质量控制的有效方法,而不同批次丹红注射液中有效成分含量存在不同程度差异。

English Summary:

To determine the content of salvianolic acid hydroxy safflower yellow A(salvianolic acid A)，salvianolic acid B，salvianolic acid sodium，protocatechuic aldehyde，caffeic acid and rosmarinic acid in Danhong injection by high performance liquid chromatography(HPLC).Methods:The chromatographic conditions were determined by C18 column(type Eclipse XDB).The length of the column was 250 mm，the diameter of the packing particles in the column was 5 micron，and the inner diameter of the column was 46 mm.A binary system of acetonitrile(A phase)and 01% phosphoric acid aqueous solution(B phase)was used for gradient elution.HPLC was applied to the analysis of pharmaceutical components.The DAD detector in the HPLC system can automatically record the spectra of the corresponding components and wavelengths of chromatographic peaks in the process of chromatographic analysis.The method of HPLC was rigorous，including linear relationship，precision，repeatability，stability and sample recovery.Based on the rigorous method，the content of Danhong injection was determined.Results:1)The UV-Vis spectrophotometer was used to detect 6 reference substances，and the detection wavelength was 280 nm，which could be used to determine salvianolic acid sodium，protocatechuic aldehyde，salvianolic acid B and salvianolic acid A，while the detection wavelength was 330 nm，which could be used to determine caffeic acid and rosmarinic acid.2)Linear regression equation，correlation coefficient and linear range were：salvianolic acid A：Y=162X+769，0999 9，3362～3 36200 μg/mL; salvianolic acid B：Y=8431X+1884，0999 8，221～2 21000 μg/mL; salvianolic acid sodium：Y=3740X+69608，0999 1，1178～1 17800 μg/mL; protocatechuic aldehyde：20345X+2102 μg/mL; Caffeic acid：Y=118453X+248，0999 7，005～510 μg/mL; rosmarinic acid：Y=20304X+6593，0999 9，108～10800 μg/mL.3)The average recoveries of salvianolic acid A，salvianolic acid B，salvianolic acid sodium，protocatechuic aldehyde，caffeic acid and rosmarinic acid were 10020%，10103%，9901%，10087%，10043%，9874% and RSD respectively.The recoveries of the samples were 129%，165%，129%，1035%，132% and 184% respectively，which indicated that the method of HPLC was reliable.4)The HPLC chromatograms of mixed reference solution and Danhong injection solution showed that the six components in Danhong injection solution were well separated from other coexisting peaks，and the contents of components in 3 different batches of Danhong injection were different in varying degrees.Conclusion:HPLC is a simple，accurate，stable and reproducible method for the quality control of Danhong injection.The contents of active ingredients in different batches of Danhong injection are different.

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