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71.
采用超高速液相色谱-质谱(UFLC-MS)研究了吴茱萸醇提取物中入血小分子化合物的体内药代动力学过程. 同时对UFLC-MS 生物样品分析方法进行包括特异性、 线性、 精密度、 准确度、 稳定性、 基质效应和回收率等考察, 结果表明, 该方法稳定可靠, 且醇提取物中10个生物碱类化合物均被胃肠道快速吸收, 并且多数化合物血药浓度在1~2 h左右达到峰值. 将吸收入血的10个生物碱类化合物与乙酰胆碱酯酶和丁酰胆碱脂酶进行柔性分子对接及构效关系分析, 发现其中活性最高的为去氢吴茱萸碱、 吴茱萸碱、 吴茱萸次碱和吴茱萸酰胺Ⅰ 4个吲哚型生物碱, 它们与乙酰胆碱酯酶的对接打分均在-46.02 kJ/mol以下; 与丁酰胆碱脂酶对接打分均在-41.84 kJ/mol以下. 吴茱萸碱、 吴茱萸次碱、 去氢吴茱萸碱和吴茱萸酰胺可能是以乙酰胆碱酯酶和丁酰胆碱脂酶为靶点的胆碱酯酶抑制剂前体化合物. 相似文献
72.
超临界CO_2萃取连翘挥发油的正交试验和GC-MS分析 总被引:17,自引:0,他引:17
采用正交试验法对超临界CO2萃取连翘挥发油的条件进行了研究;结果显示最佳萃取条件为萃取压力30MPa,萃取温度35℃,解析压力6.7MPa,解析温度50℃,粉碎度0.55mm;按对结果的影响大小依次排列为萃取温度,粉碎度,萃取压力,解析压力,解析温度;用气相色谱-质谱联用技术测定了最佳萃取条件所得连翘挥发油的化学成分,从中鉴定出21种成分,并测定了其相对含量,主要成分为α-蒎烯、β-蒎烯、萜品醇-4、α-萜品醇、苯甲醇等。 相似文献
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The components of crude and processed Fructus Corni were investigated by means of electrospray ionization-tandem mass spectrometry(ESI-MSn) technique in the negative ion mode. Compared with those of crude Fructus Corni, the chemical components of the processed Fructus Corni were changed both in quality and in quantity.From the ESI-MS spectra of the crude and processed Fructus Corni, six peaks were selected to establish the characteristic ESI-MS peaks. Several factors in the processing procedure were examined. The experimental results demonstrate that the chemical reactions that occurred in the processing procedure can be used for the elucidation of the processed mechanism of Fructus Corni, which is regularly affected by the processing conditions. The present article provides both the chemistry evidence for the understanding of the processing procedure of Fructus Corni and the specific methodology for the research of the processing procedure and quality identification of traditional Chinese medicine. 相似文献
76.
Qualitative analysis of Psoraleae Fructus by HPLC‐DAD/TOF‐MS fingerprint and quantitative analysis of multiple components by single marker 下载免费PDF全文
《Biomedical chromatography : BMC》2018,32(2)
A variety of bioactive substances may account for the recognized efficacy and wide clinical application of Psoraleae Fructus in China. A high‐performance liquid chromatography–diode array detector (HPLC‐DAD) fingerprint method was developed to present the comprehensive phytochemical profile of the crude drug. Thirteen major compounds were separated and identified by HPLC coupled with time‐of‐flight mass spectrometry (HPLC/TOF‐MS), namely psoralenoside (PO), isopsoralenoside (IPO), psoralen (PS), isopsoralen (IPS), neobavaisoflavone (NBF), bavachin (BC), corylin (CN), bavachromene (BCM), psoralidin (PD), isobavachalcone (IBC), bacachinin (BCN), corylifol A (CA) and bakuchiol (BK). Then quantitative analysis of multiple components by single marker (QAMS) was applied in content determination of PO, IPO, PS, IPS, BC, IBC, BCN, CA and BK, with NBF as the internal standard. The calculation results indicated no significant difference from the traditional external standard method (p > 0.05, RSD < 2.62%), suggesting that QAMS is a reliable and convenient method for content determination of multiple chemical compositions, especially when there is a shortage of reference substances. In conclusion, simultaneous qualitative and quantitative analysis of Psoraleae Fructus may be fulfilled through the newly proposed method of QAMS combined with HPLC‐DAD/TOF‐MS fingerprint. 相似文献
77.
电喷雾解吸电离质谱快速测定吴茱萸中生物碱 总被引:5,自引:0,他引:5
生物碱是许多中草药的活性有效成分,其含量的多少和种类的差异是导致中草药品质差异的重要因素.本文利用电喷雾解吸电离质谱(DESI-MS)能够在不需要样品预处理的前提下进行复杂基体样品分析的特点,采用酸性甲醇-水混合溶液作为喷雾试剂,在优化了的实验条件下快速获得了吴茱萸的DESI-MS指纹谱图,然后利用串联质谱对其中有重要活性的5种生物碱进行了结构鉴定.实验表明,基于固体表面解吸电离质谱分析的方法不需要萃取-分离手续,单个样品测定时间不超过1.5 min,大幅度提高了分析速度,有望在药品品质的在线监测和工艺过程控制中发挥重要作用. 相似文献
78.
Yucheng Wang Keyu Feng Mengrong Li Lifeng Han Weiqiang Wang Dandan Si Xiaopeng Chen Wenzhi Yang Xiumei Gao Erwei Liu 《Biomedical chromatography : BMC》2020,34(7):e4833
The identification and quantization of traditional Chinese medicine (TCM) are a challenge for researchers and industry. Using untargeted analytical methods, the in vivo detection and identification of TCM compounds are difficult because of the significant interference of endogenous substances. Fortunately, the ongoing development of new analytical technologies, especially Q-Orbitrap–MS, offers some solutions. Our team developed a holistic MS method, combining untargeted data-dependent MS2 (dd-MS2) modes to extensively identify TCM prototypes in vivo. The method was successfully applied to the analysis of Ligustri Lucidi Fructus (LLF). LLF is a widely used TCM with a remarkable nourishing effect on the liver and kidney. In the study, we aimed to identify the prototypes in rat plasma after oral administration of LLF extract. Following separation on an HSS T3 column, LLF extract and rat plasma were performed in untargeted dd-MS2 mode. Forty-seven compounds were characterized in rats plasma as prototypes of LLF extract. Furthermore, seven major prototypes were chosen as pharmacokinetic markers to investigate LLF's pharmacokinetic properties. The results provides comprehensive determination of compounds in LLF both in vitro and in vivo, which is important for quality control, pharmacology studies and clinical use of LLF. 相似文献
79.
Fragmentation patterns study of iridoid glycosides in Fructus Gardeniae by HPLC‐Q/TOF‐MS/MS 下载免费PDF全文
Zhiwen Fu Rui Xue Zhixiong Li Mingcang Chen Zhaolin Sun Yiyang Hu Chenggang Huang 《Biomedical chromatography : BMC》2014,28(12):1795-1807
Iridoid glycosides (IGs), the major constituents in Fructus Gardeniae, have demonstrated various pharmacological activities, but there is no systematic chemical profile of IGs in Fructus Gardeniae in the published literature until now. Therefore, it is imperative that a rapid and sensitive high‐performance liquid chromatography coupled with quadrupole time‐of‐flight tandem mass spectrometry (HPLC‐Q/TOF‐MS/MS) method is established for comprehensive characterization of IGs in Fructus Gardeniae. Firstly, the fragmentation patterns of six known IGs were investigated and proposed and further concluded the diagnostic fragment ions and characteristic fragmentation pathways. Then, based on the summarized fragmentation patterns and the known compounds in the literatures, the other IGs in Fructus Gardeniae were identified successively. As a result, a total of 20 IGs were identified, of which three pairs of epimers were structurally characterized and differentiated. More importantly, one compound, the isoshanzhiside methyl ester, was tentatively identified as a new compound. The results of this study demonstrate the superiority of HPLC‐MS with a high‐resolution mass spectrometer for the rapid and sensitive structural elucidation of the multiple groups of constituents in Fructus Gardeniae. Copyright © 2014 John Wiley & Sons, Ltd. 相似文献
80.
A new phenolic glycoside, citrauranoside A (1), and two new monoterpenoid furocoumarins, citraurancoumarin A (2) and citraurancoumarin B (3), along with four known compounds (4–7) were isolated from the young fruit of Citrus aurantium L. The structures were elucidated by their comprehensive analysis including 1D, 2DNMR, IR and mass spectra. 相似文献