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81.
Simultaneous chemical fingerprint and quantitative analysis of Rhizoma Smilacis Glabrae by accelerated solvent extraction and high‐performance liquid chromatography with tandem mass spectrometry 下载免费PDF全文
Weiquan Dai Weiquan Zhao Fangyuan Gao Jingjing Shen Diya Lv Yunpeng Qi Guorong Fan 《Journal of separation science》2015,38(9):1466-1475
Rhizoma Smilacis Glabrae (RSG) is a well‐known herbal medicine with the homology of medicine and food. In this study, simultaneous chemical fingerprint and quantitative analysis of the bioactive flavonoid components of RSG were developed using accelerated solvent extraction and high‐performance liquid chromatography coupled with ion trap tandem mass spectrometry. The operational parameters of accelerated solvent extraction including extraction solvent, extraction temperature, static extraction time, solid‐to‐liquid ratio, and extraction cycles were optimized. Hierarchical cluster analysis, similarity analysis, and principal component analysis were performed to evaluate the similarity and variation of the samples collected from several provinces in China. Subsequently, high‐performance liquid chromatography fingerprints were established for the discrimination of 16 batches of RSG samples, and the major six flavonoids, namely, toxifolin, neoastilbin, astilbin, neoisoastilbin, isoastilbin, and engeletin were then quantitatively determined. The calibration curves for all the six analytes showed good linearity (r2 > 0.999), and the limits of detection and quantification were less than 0.10 and 0.27 μg·mL?1, respectively. Therefore, the proposed extraction and determination methods were proved to be robust and reliable for the quality control of RSG. 相似文献
82.
Development of a liquid chromatography with mass spectrometry method for the determination of gelsemine in rat plasma and tissue: Application to a pharmacokinetic and tissue distribution study 下载免费PDF全文
Shuangshuang Zhang Shuping Hu Xiangxiang Yang Jiaqi Shen Xiaoyong Zheng Kexin Huang Zheng Xiang 《Journal of separation science》2015,38(6):936-942
Gelsemine from Gelsemium elegans Benth is a potential anesthetic and analgesic agent with no physical dependence and opiate addiction. This study was aimed at developing an ultrafast liquid chromatography coupled to tandem mass spectrometry method to quantify gelsemine in rat plasma and tissues. Plasma and tissues were processed with acetonitrile precipitation, and dendrobine was chosen as the internal standard. Sample separation was performed on an ACQUITY HSS T3 column. The mobile phase consisted of acetonitrile and 0.1% formic acid aqueous solution. Multiple reactions monitoring mode was utilized to detect the compounds of interest. The mass spectrometer was operated in the positive ion mode for detection. The MS/MS ion transitions monitored were m/z 323.2→70.5 for gelsemine and 264.2→108.05 for dendrobine, respectively. The calibration curves were linear over the range of 1–500 ng/mL in all biological matrices. The lower limit of quantification for rats plasma and tissues was 1.0 ng/mL. The values for inter‐ and intraday precision and accuracy were well within the ranges acceptable (< 15%). It was successfully applied to the pharmacokinetic and tissue distribution studies of gelsemine after intravenous doses of 5, 2, and 0.5 mg/kg in rats. These data of gelsemine would be useful for clinical application and further development. 相似文献
83.
Determination of five sesquiterpenoids in Xingnaojing injection by quantitative analysis of multiple components with a single marker 下载免费PDF全文
Weidong Pan Lixin Yang Weihong Feng Limei Lin Chun Li Guofeng Gan Junhong Fan Jigao Zou Zhimin Wang Haifeng Pan 《Journal of separation science》2015,38(19):3313-3323
A quantitative analysis of multiple components with a single‐marker method was established for the simultaneous determination of five sesqutiterpenoids in Xingnaojing injection. This method was established with Xingnaojing injection determined by high‐performance liquid chromatography coupled with diode array detection. The durability and system suitability of the established method were evaluated, and the reliable relative correction factors were obtained with curdione selected as an internal reference. The contents of the five components in all Xingnaojing injections were determined by external standard method and the contents of curcumenone, curcumenol, curzerenone, and germacrone were also calculated with the obtained relative correction factors. Then, relative error was investigated to estimate the difference of the two methods. As a result, the established new method possesses good adaptability, and there is no significant difference between the two methods, except for the content of curzerenone in eight samples. To put the established method into practice, the limits of quantitation of the established method of the five components were proposed and defined. Thus, the developed methodology can also be utilized to the quality evaluation of Xingnaojing injection, in spite of the difference found in the content of curzerenone between the external standard method and the newly established method. 相似文献
84.
Determination of hexavalent chromium in traditional Chinese medicines by high‐performance liquid chromatography with inductively coupled plasma mass spectrometry 下载免费PDF全文
Peng Li Li‐min Li Jing Xia Shuai Cao Xin Hu Hong‐Zhen Lian Shen Ji 《Journal of separation science》2015,38(23):4043-4047
An analytical method that combined high‐performance liquid chromatography with inductively coupled plasma mass spectrometry has been developed for the determination of hexavalent chromium in traditional Chinese medicines. Hexavalent chromium was extracted using the alkaline solution. The parameters such as the concentration of alkaline and the extraction temperature have been optimized to minimize the interconversion between trivalent chromium and hexavalent chromium. The extracted hexavalent chromium was separated on a weak anion exchange column in isocratic mode, followed by inductively coupled plasma mass spectrometry determination. To obtain a better chromatographic resolution and sensitivity, 75 mM NH4NO3 at pH 7 was selected as the mobile phase. The linearity of the proposed method was investigated in the range of 0.2–5.0 μg L?1 (r2 = 0.9999) for hexavalent chromium. The limits of detection and quantitation are 0.1 and 0.3 μg L?1, respectively. The developed method was successfully applied to the determination of hexavalent chromium in Chloriti lapis and Lumbricus with satisfactory recoveries of 95.8–112.8%. 相似文献
85.
Leticia A. Montoya Xinggui Shen James J. McDermott Christopher G. Kevil Michael D. Pluth 《Chemical science》2015,6(1):294-300
Hydrogen sulfide (H2S) has emerged as an important biological signaling molecule in the last decade. During the growth of this field, significant controversy has arisen centered on the physiological concentrations of H2S. Recently, a monobromobimane (mBB) method has been developed for the quantification of different biologically-relevant sulfide pools. Based on the prevalence of the mBB method for sulfide quantification, we expand on this method to report the use of dibromobimane (dBB) for sulfide quantification. Reaction of H2S with dBB results in formation of highly-fluorescent bimane thioether (BTE), which is readily quantifiable by HPLC. Additionally, the reaction of sulfide with dBB to form BTE is significantly faster than the reaction of sulfide with mBB to form sulfide dibimane. Using the dBB method, BTE levels as low as 0.6 pM can be detected. Upon use of the dBB method in wild-type and CSE–/– mice, however, dBB reports significantly higher sulfide levels than those measured using mBB. Further investigation revealed that dBB is able to extract sulfur from other sulfhydryl sources including thiols. Based on mechanistic studies, we demonstrate that dBB extracts sulfur from thiols with α- or β-hydrogens, thus leading to higher BTE formation than from sulfide alone. Taken together, the dBB method is a highly sensitive method for H2S but is not compatible for use in studies in which other thiols are present. 相似文献
86.
Nan Zhang Tao Bing Xiangjun Liu Cui Qi Luyao Shen Linlin Wang Dihua Shangguan 《Chemical science》2015,6(7):3831-3838
Guanine-rich oligonucleotides (GROs) have attracted considerable attention as anticancer agents, because they exhibit cancer-selective antiproliferative activity and can form G-quadruplex structures with higher nuclease resistance and cellular uptake. Recently, a GRO, AS1411 has reached phase II clinical trials for acute myeloid leukemia and renal cell carcinoma. The antiproliferative activity of GROs has been associated with various protein targets; however the real mechanisms of action remain unclear. In this study, we showed evidence that antiproliferative activity of GROs (including AS1411) is mainly contributed by the cytotoxicity of their guanine-based degradation products, such as monophosphate deoxyguanosine (dGMP), deoxyguanosine (dG) and guanine. The GROs with lower nuclease resistance exhibited higher antiproliferative activity. Among nucleotides, nucleosides and nucleobases, only guanine-based compounds showed highly concentration-dependent cytotoxicity. Our results suggest that it is necessary to reconsider the cancer-selective antiproliferative activity of GROs. Since guanine-based compounds are endogenous substances in living organisms, systematic studies of the cytotoxicity of these compounds will provide new information for the understanding of certain diseases and offer useful information for drug design. 相似文献
87.
Jiangwei Tian Jinfeng Zhou Zhen Shen Lin Ding Jun-Sheng Yu Huangxian Ju 《Chemical science》2015,6(10):5969-5977
This work reports a newly designed pH-activatable and aniline-substituted aza-boron-dipyrromethene as a trifunctional photosensitizer to achieve highly selective tumor imaging, efficient photodynamic therapy (PDT) and therapeutic self-monitoring through encapsulation in a cRGD-functionalized nanomicelle. The diethylaminophenyl is introduced in to the structure for pH-activatable near-infrared fluorescence and singlet oxygen (1O2) generation, and bromophenyl is imported to increase the 1O2 generation efficiency upon pH activation by virtue of its heavy atom effect. After encapsulation, the nanoprobe can target αvβ3 integrin-rich tumor cells via cRGD and is activated by physiologically acidic pH for cancer discrimination and PDT. The fascinating advantage of the nanoprobe is near-infrared implementation beyond 800 nm, which significantly improves the imaging sensitivity and increases the penetration depth of the PDT. By monitoring the fluorescence decrease in the tumor region after PDT, the therapeutic efficacy is demonstrated in situ and in real time, which provides a valuable and convenient self-feedback function for PDT efficacy tracking. Therefore, this rationally designed and carefully engineered nanoprobe offers a new paradigm for precise tumor theranostics and may provide novel opportunities for future clinical cancer treatment. 相似文献
88.
Rui Shen Zhiqing Meng Chuangyin Dang Min Jiang 《Numerical Functional Analysis & Optimization》2017,38(11):1473-1489
In this paper, an algorithm of barrier objective penalty function for inequality constrained optimization is studied and a conception–the stability of barrier objective penalty function is presented. It is proved that an approximate optimal solution may be obtained by solving a barrier objective penalty function for inequality constrained optimization problem when the barrier objective penalty function is stable. Under some conditions, the stability of barrier objective penalty function is proved for convex programming. Specially, the logarithmic barrier function of convex programming is stable. Based on the barrier objective penalty function, an algorithm is developed for finding an approximate optimal solution to an inequality constrained optimization problem and its convergence is also proved under some conditions. Finally, numerical experiments show that the barrier objective penalty function algorithm has better convergence than the classical barrier function algorithm. 相似文献
89.
Xuan Shen Xiaohong Xia Weichun Ye Yongling Du Chunming Wang 《Journal of Solid State Electrochemistry》2017,21(2):409-417
Hexagram-like CoS-MoS2 composites were prepared on indium tin oxide (ITO) conductive glasses via cyclic voltammetry electrodeposition using Co(NO3)2 and (NH4)2MoS2 as precursors and tested for application in hydrogen evolution reaction (HER). The structure of CoS-MoS2 composites was characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), and X-ray photoelectron spectrum (XPS). Electrochemical characterizations indicate that CoS-MoS2 composites exhibit more excellent catalytic activity and stability than MoS2. Compared with pure MoS2, the hexagram-like CoS-MoS2 composites with increased specific surface area improved the density of exposed active sites, and the Co binding S edges in CoS-MoS2 composites promote the number of highly catalytic edge sites and decreased the binding energy △G H. Moreover, the effects of different substrates on the CoS-MoS2 composites were also investigated. Our further understanding of this highly active hydrogen evolution catalyst can facilitate the development of economical electrochemical hydrogen production systems. 相似文献
90.