天冬饮片与标准汤剂的质量评价方法探索  

Analysis on Quality Evaluation Methods of Asparagi Radix Decoction Pieces and Its Standard Decoction

作　　者：靳如娜 郝丽霞 王涛[1] 吴红华[1] 代云桃[2] 石守刚 黄正军 JIN Ru-na;HAO Li-xia;WANG Tao;WU Hong-hua;DAI Yun-tao;SHI Shou-gang;HUANG Zheng-jun(Institute of Traditional Chinese Medicine(TCM),Tianjin University of TCM,Tianjin 300193,China;Institute of Chinese Materia Medica,China Academy of Chinese Medical Sciences,Beijng 100700,China;Sunflower Pharmaceutical Group(Xiangyang)Longzhong Co.Ltd.,Xiangyang 441003,China)

机构地区：[1]天津中医药大学中医药研究院,天津300193 [2]中国中医科学院中药研究所,北京100700 [3]葵花药业集团(襄阳)隆中有限公司,湖北襄阳441003

出　　处：《中国实验方剂学杂志》2020年第17期111-118,共8页Chinese Journal of Experimental Traditional Medical Formulae

基　　金：中国中医科学院中药研究所古代经典名方的开发研究项目(H2018026)。

摘　　要：目的:建立天冬饮片及其标准汤剂的质量评价方法。方法:制备10批天冬标准汤剂。采用高效液相色谱-蒸发光散射检测法(HPLC-ELSD),以乙腈-水为流动相梯度洗脱,建立天冬饮片、标准汤剂的指标成分含量测定方法以及天冬饮片的指纹图谱检测方法。采用UHPLC-LTQ-Orbitrap-MS/MS对指纹图谱中主要共有峰进行成分指认,以乙腈-0.1%甲酸水溶液为流动相,电喷雾离子源(ESI),正、负离子模式扫描,检测范围m/z 100~1400。结果:天冬饮片、标准汤剂中原薯蓣皂苷与原新薯蓣皂苷的总质量分数分别为0.41%~0.72%和0.33%~0.59%,这2个成分的转移率73.6%~98.3%。天冬标准汤剂的出膏率59.0%~73.0%,pH 4.9~5.6。天冬饮片的HPLC指纹图谱中呈现了10个共有峰,且均为皂苷类成分,包括原新薯蓣皂苷,原薯蓣皂苷,天冬皂苷甲及其同分异构体,甲基原薯蓣皂苷,asparagoside F,(25R)-26-O-β-D-葡萄吡喃糖基-呋甾-5,20-二烯-3β,26-二醇-3-O-[α-L-鼠李吡喃糖基(1→2)]-[β-D-葡萄吡喃糖基(1→4)-α-L-鼠李吡喃糖基(1→4)]-β-D-葡萄吡喃糖苷,26-O-β-D-葡萄吡喃糖基-呋甾-20(22)-烯-3β,26-二醇-3-O-[α-L-鼠李吡喃糖基(1→2)]-[α-L-鼠李吡喃糖基(1→4)]-β-D-葡萄吡喃糖苷,伪原薯蓣皂苷,aspacochioside C。结论:建立了天冬饮片及其标准汤剂的质量评价方法,且建立的方法稳定可行,可为含天冬制剂的质量评价及控制提供参考。Objective:To establish the quality evaluation methods of Asparagi Radix decoction pieces and its standard decoction.Method:Ten batches of Asparagi Radix standard decoction were prepared.High performance liquid chromatography-evaporative light scattering detection method(HPLC-ELSD)was established for the determination of protodioscin and protoneodioscin in Asparagi Radix decoction pieces and its standard decoction,and the fingerprint detection of Asparagi Radix decoction pieces with acetonitrile-water as mobile phase for gradient elution.UHPLC-LTQ-Orbitrap-MS/MS was used to identify ten main common peaks in the fingerprint with acetonitrile-0.1%formic acid solution as mobile phase for gradient elution,electrospray ionization(ESI)and positive and negative ion mode scanning were employed,the detection range was m/z 100-1400.Result:The total content of protodioscin and protoneodioscin in Asparagi Radix decoction pieces was0.41%-0.72%,and their total content in Asparagi Radix standard decoction was 0.33%-0.59%,the transfer rate of these two components was 73.6%-98.3%.The dry extract yield of the standard decoction was 59.0%-73.0%,and its pH was 4.9-5.6.There were 10 common peaks in the fingerprint,and all of them were saponins,including protoneodioscin,protodioscin,aspacochioside A and its isomer,methyl protodioscin,asparagoside F,(25 R)-26-O-β-D-glucopyranosyl-furostan-5,20-diene-3β,26-diol-3-O-[α-L-rhamnopyranosyl(1→2)]-[β-D-glucopyranosyl(1→4)-α-L-rhamnopyranosyl(1→4)]-β-D-glucopyranoside,26-O-β-D-glucopyranosylfurostan-20(22)-ene-3β,26-diol-3-O-[α-L-rhamnopyranosyl(1→2)]-[α-L-rhamnopyranosyl(1→4)]-β-Dglucopyranoside,pseudodiosgenin,aspacochioside C.Conclusion:In this paper,the quality evaluation methods of Asparagi Radix decoction pieces and its standard decoction are established,and these methods are stable and feasible,which can provide reference for the quality control of pharmaceutical preparations containing Asparagi Radix.

关 键 词：天冬 饮片 标准汤剂 原薯蓣皂苷 原新薯蓣皂苷 指纹图谱 高效液相色谱-蒸发光散射检测法(HPLC-ELSD) 

分 类 号：R22[医药卫生—中医基础理论] R28[医药卫生—中医学]