SFC和UPLC方法用于丹参饮片中多成分研究  

Multiple components analysis of Salvia Miltiorrhiza decoction pieces by SFC and UPLC

作　　者：张光华 付龙[4] 王京辉 宋彬彬 郭伟[1,3] 张琳培 钱忠直 ZHANG Guang-hua;FU Long;WANG Jing-hui;SONG Bin-bin;GUO Wei;ZHANG Lin-pei;QIAN Zhong-zhi(ChP-Waters Joint Open Laboratory,Beijing 100061,China;Beijing Institute for Drug Control,Beijing Key Lab.Analysis and Evaluation on Chinese Medicine,Beijing 102206,China;Chinese Pharmacopeia Commission,Beijing 100061,China;R&D Center of Livzon Pharmaceutical Group,Zhuhai 519090,China;China Z.Pharmaceutical Productivity Centre,Beijing 101111,China)

机构地区：[1]ChP-Waters联合开放实验室,北京100061 [2]北京市药品检验所,中药成分分析与生物评价北京市重点实验室,北京102206 [3]国家药典委员会,北京100061 [4]丽珠医药集团研究院,珠海519090 [5]中关村现代医药生产力促进中心,北京101111

出　　处：《药物分析杂志》2020年第5期940-947,共8页Chinese Journal of Pharmaceutical Analysis

基　　金：国家药典委员会药品标准制修订研究课题(编号:2018Y005)。

摘　　要：目的:建立SFC-PDA法同时检测丹参饮片中4个脂溶性丹参酮类成分,以及UPLC法同时测定丹参饮片中3个水溶性丹酚酸类成分,以7个成分的测定结果综合评价丹参饮片的质量。方法:采用SFC-PDA法,使用Viridis■HSS SB C18100A(3.0 mm×100 mm,1.8μm)色谱柱,以二氧化碳(A)-[正庚烷-异丙醇(8∶2)(B)]为流动相,梯度洗脱,流速1.5 mL·min^-1,柱温45℃,背压13.8 MPa;采用UPLC-PDA法,使用BEH Shield RP(2.1 mm×100 mm,1.7μm)色谱柱,以乙腈(A)-0.1%磷酸溶液(B)为流动相,梯度洗脱,流速0.4 mL·min^-1,柱温30℃。结果:在建立的色谱条件下,丹参饮片中7个主要成分在各自的液相系统中分离完全,线性良好,精密度、重复性、稳定性及回收率实验结果均符合含量测定要求,同时还比较了用HPLC和SFC 2种方法测定脂溶性成分时的仪器灵敏度,结果为一个数量级。结论:SFC方法快速简便、结果准确,在节省溶剂、减少环境污染的方面具有独特优势,同时采用UPLC方法测定水溶性成分,2种方法可用于丹参饮片的质量分析,同时大大降低检测成本。Objective:To evaluate the quality of Salvia Miltiorrhiza decoction pieces from difference sources,methods for determining 7 components were established.Among which,lipid-soluble tanshinone components were determined by(SFC-PDA),and 3 water-soluble salvianolic acid components were determined by UPLC.Methods:The SFC-PDA analysis was performed on Viridis■HSS SB C18100 A(3.0 mm×100 mm,1.8μm)column.The mobile phase was Carbon dioxide-n-heptane-isopropanol(8∶2)with isocratic elution mode at a flow rate of 1.5 m L·min^-1.The column temperature was controlled at 45℃and the ABPR pressure was 13.8 MPa.The UPLC-PDA analysis was performed on BEH Shield RP(2.1 mm×100 mm,1.7μm)column,The mobile phase consisted of acetonitrile-0.1%phosphoric acid with gradient elution at a flow rate of 0.4 m L·min^-1.The column temperature was controlled at 30℃.Results:7 main components in Salvia Miltiorrhiza decoction pieces were well separated by SFC and UPLC respectively.Results of linearity,repeatability,stability and recovery met the accept criteria of assay.The sensitivity of fat-soluble components and water-soluble components were comparable in HPLC and SFC system.Conclusion:The SFC method rapid,simple and accurate,which possesses the advantage of solvent saving and environmental friendly.At the same time,the UPLC method is used to determine the water-soluble components.The two methods can be used for analysis the quality of Salvia Miltiorrhiza decoction pieces,and reduce the detection cost remarkably.

关 键 词：超临界流体色谱 超高效液相色谱 含量测定 丹参饮片 丹参酮类成分 丹酚酸类成分 

分 类 号：R917[医药卫生—药物分析学]