一测多评法同时测定丹参药材中8种水溶性成分含量  

Simultaneous Determination of Eight Water-Soluble Components in Salviae Miltiorrhizae Radix et Rhizoma by QAMS

作　　者：陈雪琴 贾文江 周仔莉 李鹏 贾卫 柯园 王敏珍 张跃进[3] CHEN Xueqin;JIA Wenjiang;ZHOU Zili;LI Peng;JIA Wei;KE Yuan;WANG Minzhen;ZHANG Yuejin(Shangluo Pharmaceutical Inspection Institute,Shangluo,Shaanxi,China 726000;Shangluo Agricultural Science Research Institute,Shangluo,Shaanxi,China 726000;Northwest A&F University,Xianyang,Shaanxi,China 712100)

机构地区：[1]陕西省商洛市药品检验所,陕西商洛726000 [2]陕西省商洛市农业科学研究所,陕西商洛726000 [3]西北农林科技大学,陕西咸阳712100

出　　处：《中国药业》2023年第10期89-94,共6页China Pharmaceuticals

基　　金：陕西省商洛市科技计划项目[2020-Y-0005];广西壮族自治区壮瑶药重点实验室开放课题[GXZYKF2020A-12]。

摘　　要：目的建立检测丹参药材中8种水溶性成分含量的一测多评(QAMS)法。方法采用高效液相色谱法,色谱柱为Agilent 5 TCC18柱(250 mm×4.6 mm,5μm),流动相为乙腈-0.2%磷酸溶液(20∶80,V/V),流速为1.1 mL/min,检测波长为286 nm,柱温为30℃,进样量为20μL。以丹酚酸B为内标,计算药材样品中其余7个成分的相对校正因子及含量,并与外标法的检测结果比较。结果丹参素钠、原儿茶醛、咖啡酸、丹酚酸F、迷迭香酸、紫草酸、丹酚酸B、丹酚酸A进样量分别在55.257~1381.425 ng、12.848~321.210 ng、19.3418~483.5450 ng、24.5~612.5 ng、94.176~2354.400 ng、105.84~2646.00 ng、75.831~1895.775 ng、13.524~338.100 ng范围内与峰面积线性关系良好(R2>0.9990);精密度、稳定性、重复性试验结果的RSD均小于1.5%;平均加样回收率为98.94%~102.43%,RSD均小于1.5%(n=6)。7个成分的相对校正因子在不同型号仪器(不同色谱柱)、柱温、流速条件下的RSD均小于1.0%。QAMS法与外标法测得7个成分的含量无显著差异(P>0.05)。结论所建立的QAMS法可用于同时测定丹参药材中8种水溶性成分的含量,方便快速、准确可靠且重复性好,可为丹参药材的质量控制提供参考。Objective To establish a quantitative analysis of multi-components by single-marker(QAMS)method for the simultaneous determination of eight water-soluble components in Salviae Miltiorrhizae Radix et Rhizoma.Methods High-performance liquid chromatography(HPLC)was adopted,and the chromatographic column was Agilent 5 TC-C18 column(250 mm×4.6 mm,5μm),the mobile phase was acetonitrile-0.2%phosphoric acid solution(20∶80,V/V),the flow rate was 1.1 mL/min,the detection wavelength was 286 nm,the column temperature was 30℃,and the injection volume was 20μL.With salvianolic acid B as the internal standard,the relative correction factor and content of the other seven components in medicinal material samples were calculated,and the detection results were compared with those of the external standard method.Results The linear ranges of sodium Danshensu,protocatechualdehyde,caffeic acid,salvianolic acid F,rosmarinic acid,lithospermic acid,salvianolic acid B and salvianolic acid A were 55.257-1381.425 ng,12.848-321.210 ng,19.3418-483.5450 ng,24.5-612.5 ng,94.176-2354.400 ng,105.84-2646.00 ng,75.831-1895.775 ng,and 13.524-338.100 ng(R2>0.9990),respectively.The RSDs of precision,stability,and repeatability tests were all lower than 1.5%.The average recoveries of eight components were in the range of 98.94%-102.43%,and the RSDs were lower than 1.5%(n=6).The RSDs of the relative correction factors for the seven components under different types of instruments(different chromatographic columns),column temperatures,and flow rates were all lower than 1.0%.The content of seven components determined by the QAMS method and external standard method had no significant difference(P>0.05).Conclusion The established QAMS method can simultaneously determine the content of eight water-soluble components in Salviae Miltiorrhizae Radix et Rhizoma,which is convenient,rapid,accurate,reliable and repeatable,and it can provide a reference for the quality control of Salviae Miltiorrhizae Radix et Rhizoma.

关 键 词：丹参 一测多评法 水溶性成分 高效液相色谱法 相对校正因子 质量控制 

分 类 号：R917[医药卫生—药物分析学] R927[医药卫生—药学]