摘要
目的使用超高效液相色谱-二极管阵列检测器检测法(UHPLC-DAD)和解吸电喷雾电离-离子化质谱成像技术(desorption electrospray ionization-mass spectrometry imaging,DESI-MSI)对15批芍药甘草汤(Shaoyao-Gancao-Decoction,SGD)物质基准和对应实物进行分析,考察DESI-MSI在经典名方SGD质量控制中的优势。方法以SGD为研究模型,采用传统UHPLC-DAD法建立物质基准指纹图谱,并对SGD指标成分(芍药苷、甘草苷、甘草酸)含量、出膏率进行考察。同时,以芍药甘草汤对应实物冻干粉为研究载体,将其复溶后点样于定性滤纸,并固定于载玻片制成样品,以甲醇-甲酸(1000∶1)为喷雾溶剂,体积流量3μL/min;扫描范围m/z 100~1200;空间分辨率300μm;喷雾气(N2)压力0.5 MPa;离子源温度120℃,采用正负离子全扫描样本。结果DESI-MSI法能检测到SGD指标成分芍药苷、甘草苷、甘草酸以及共有峰成分芍药内酯苷等。同时,DESI-MSI法还能检测到来自甘草、白芍的甘草皂苷G2、甘草皂苷J2、没食子酸、柠檬酸、对羟基苯甲酸等11种成分,并对其相对含量进行直观呈现,定性分析能力远强于UHPLC-DAD法。结论基于DESI-MSI技术无需进行复杂的样品前处理,可以在无对照品情况下进行复杂样品的定性、相对含量分析,灵敏度高,分析能力强,可以作为经典名方物质基准、对应实物及配方颗粒样品的质控研究方法。
Objective Using ultra-high performance liquid chromatography with diode array detection(UHPLC-DAD) and desorption electrospray ionization-mass spectrometry imaging(DESI-MSI) to analyze 15 batches of Shaoyao Gancao Decoction(SGD) substance benchmark and lyophilized powder in order to investigate the advantages of DESI-MSI in quality control of famous classical formulas. Methods Taking SGD as the research model, fingerprints of the substance benchmark were established by UHPLC-DAD, and the content of index components(paeoniflorin, liquiritin, glycyrrhizic acid) and the yield of dry extract were also investigated. Meanwhile, as the research carrier, the lyophilized powder corresponding to SGD was dissolved in methanol and dotted on qualitative filter paper with quantitative capillary, and fixed it on the slide to make samples. The samples were analyzed on a DESI-MSI system in positive and negative ion mode with methanol-formic acid(1 000∶1, flow rate of 3 μL/min) as spray solvent, N2 as spray gas(pressure of 0.5 MPa). The scanning range was m/z 100—1 200, the spatial resolution was 300 μm, the ion source temperature was 120 ℃. Results DESI-MSI can detect not only the index components of paeoniflorin, liquiritin, glycyrrhizic acid, but also the common peaks of albiflorin. At the same time, DESI-MSI could detect 11 other components from Glycyrrhizae Radix et Rhizoma and Paeoniae Radix Alba, such as licoricesaponin G2, licoricesaponin J2, gallic acid, citric acid, p-hydroxybenzoic acid, and present their relative content visually. The qualitative analysis ability of DESI-MSI was much better than UHPLC-DAD. Conclusion DESI-MSI can be used as the quality control method for substance benchmark and lyophilized powder and dispensing granules of classical famous formulas with advantages of high sensitivity, strong analytical ability, no complex sample pretreatment, qualitative and relative content analysis of complex samples without reference substance.
作者
曲缘章
孙博
朱广伟
马生军
万林春
李雅静
郭杰
李刚
杨林勇
李宝国
QU Yuan-zhang;SUN Bo;ZHU Guang-wei;MA Sheng-jun;WAN Lin-chun;LI Ya-jing;GUO Jie;LI Gang;YANG Lin-yong;LI Bao-guo(Institute of Chinese Materia Medica,China Academy of Chinese Medical Sciences,Beijing 100700,China;Shandong University of Traditional Chinese Medicine,Jinan 250355,China;Harbin University of Commerce,Harbin 150076,China;School of Food Sciences and Pharmacy,Xinjiang Agriculture University,Urumqi 830052,China;Jiangxi Institute for Drug Control,Nanchang 330029,China;Beijing University of Chinese Medicine,Beijing 100102,China;Tianjin University of Traditional Chinese Medicine,Tianjin 300193,China;China Medico Corporation,Tianjin 300301,China)
出处
《中草药》
CAS
CSCD
北大核心
2020年第13期3433-3443,共11页
Chinese Traditional and Herbal Drugs
基金
国家重点研发计划项目(2018YFC1706500)
国家“重大新药创制”科技重大专项(2018ZX09721005)
中央级公益性科研院所基本科研业务费专项资金资助(ZXKT17034)。
关键词
经典名方
芍药甘草汤
解吸电喷雾电离-离子化质谱成像技术
UHPLC-DAD
物质基准
质量标准
质量控制
芍药苷
甘草苷
甘草酸
芍药内酯苷
甘草皂苷G2
甘草皂苷J2
没食子酸
柠檬酸
对羟基苯甲酸
classical famous formulas
Shaoyao Gancao Decoction(SGD)
desorption electrospray ionization-mass spectrometry imaging(DESI-MSI)
UHPLC-DAD
substance benchmark
quality standard
quality control
paeoniflorin
liquiritin
glycyrrhizic acid
albiflorin
licoricesaponin G2
licoricesaponin J2
gallic acid
citric acid
p-hydroxybenzoic acid