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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
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为了准确测定黄精中稀土元素的含量,采用电感耦合等离子体质谱(ICP-MS)法同时测定黄精中15种稀土元素(La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu)的含量,进而绘制稀土元素指纹图谱,以稀土元素含量的平均值构建黄精稀土元素标准指纹图谱,作为鉴定黄精中药材的参考依据。黄精样品采用微波消解法处理后,通过在线引入内标溶液,采用ICP-MS法测定15种稀土元素的含量,采用OriginPro 2021绘制稀土元素指纹图谱和进行主成分分析,采用SPSS 26.0进行聚类分析。15种稀土元素的线性关系、重复性、精密度良好,平均加标回收率在97.0%~103.3%,相对标准偏差小于等于1.74%。黄精中Ce、La、Nd含量相对较高,Ce含量为53.02~2004.58 μg/kg,位居第一。聚类分析和主成分分析结果表明,样品聚为2类,同一产地的样品能够较好地聚在一起。黄精药材中15种稀土元素的指纹图谱具有相似的分布形态,具有较强的特征性和一致性,相似度均大于0.950。该方法操作简单,准确可靠,能满足实验分析要求,可为黄精的质量控制和药理研究提供参考;建立的指纹图谱可用于黄精的鉴别。 相似文献
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《Analytical letters》2012,45(14):2210-2219
A new and rapid method was developed for simultaneous determination of mangiferin, neomangiferin, timosaponin A-III, and C in Rhizoma Anemarrhenae using rapid resolution liquid chromatography coupled with triple quadrupole mass spectrometry. The analysis was performed on an Eclipse Plus C18 column (I.D. 4.6 × 100 mm, 3.5 μm). Electrospray ionization–tandem interface in the negative mode was employed prior to mass spectrometric detection. Quantitation was based on multiple reaction monitoring (MRM) for determination. Limits of detection (LODs) ranged from 0.7 to 3 pg. The average recoveries ranged from 98.16 to 100.7% with RSDs ≤ 2.03%. The established method was validated, sensitive, and reliable. 相似文献
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Xiaoxiao Wang Yixin Yao Chang An Xi Li Fangtao Xiang Yangli Dong Maosen Li 《Electrophoresis》2020,41(18-19):1606-1616
Chuanxiong Rhizoma is a commonly used in traditional Chinese medicine. Chuanxiong Rhizoma is widely distributed in Sichuan province, China, including the cities of Dujiangyan, Pengzhou, Meishan, Qionglai, and Shifang. However, reports on the comparisons of quality of Chuanxiong Rhizoma of different production origins are limited. Therefore, an ultra-HPLC with triple quadrupole MS method was developed for the determination of 20 bioactive components (12 aromatic acids and eight phthalides) in 36 samples from different production origins and further assessed its quality. The contents of these 20 constituents of samples were analyzed by hierarchical cluster analysis and orthogonal partial least squares discrimination analysis; the result indicated that Chuanxiong Rhizoma of different production origins had some differences. Thirteen constituents of quality difference markers were acquired by variable importance for the project. Furthermore, the sum of the contents of these quality difference markers was different from various production origins of Chuanxiong Rhizoma. Meanwhile, Z-ligustilide and senkyunolide A as main constituents of quality difference markers, the rate of various production origins of Chuanxiong Rhizoma was different. This study provides a foundation for the quality assessment of Chuanxiong Rhizoma. 相似文献
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High‐expression β1 adrenergic receptor/cell membrane chromatography method based on a target receptor to screen active ingredients from traditional Chinese medicines 下载免费PDF全文
Yuan Yue Hui Xue Xin Wang Qian Yang Yanhong Song Xiaoni Li 《Journal of separation science》2014,37(3):244-249
β‐Adrenergic receptors are important targets for drug discovery. We have developed a new β1‐adrenergic receptor cell membrane chromatography (β1AR‐CMC) with offline ultra‐performance LC (UPLC) and MS method for screening active ingredients from traditional Chinese medicines. In this study, Chinese hamster ovary‐S cells with high β1AR expression levels were established and used to prepare a cell membrane stationary phase in a β1AR‐CMC model. The retention fractions were separated and identified by the UPLC–MS system. The screening results found that isoimperatorin from Rhizoma et Radix Notopterygii was the targeted component that could act on β1AR in similar manner of metoprolol as a control drug. In addition, the biological effects of active component were also investigated in order to search for a new type of β1AR antagonist. It will be a useful method for drug discovery as a leading compound resource. 相似文献
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Screening of bioactive compounds in Rhizoma Polygoni Cuspidati with hepatocyte membranes by HPLC and LC–MS 下载免费PDF全文
A new method employing HPLC, LC–MS, and hepatocyte membranes for the screening of bioactive compounds in traditional Chinese medicines (TCMs) has been proposed. We hypothesized that exposure of the TCM extracts to hepatocyte membranes should decrease the concentration of membrane‐permeable compounds in the solution. Using this approach, the permeability of the compounds in Rhizoma Polygoni Cuspidati was investigated. By comparing chromatograms of samples prepared both before and after interaction with hepatocyte membranes, seven permeable compounds of Rhizoma Polygoni Cuspidati were identified. Additionally, it was found that piceid, resveratrol, emodin‐8‐β‐d‐glucoside, physcion‐8‐β‐d‐glucoside, aloe‐emodin, emodin, and physcion combined specifically with hepatocyte membranes, which might indicate a useful approach for revealing the antiatherosclerotic effects of Rhizoma Polygoni Cuspidati. Therefore, the proposed method could be a good approach to predict the potential bioactivities of multiple compounds in TCMs simultaneously. Based on the significance of these results, this method could be a novel approach for identifying potentially bioactive components in other TCMs. 相似文献
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The effect of chromatographic conditions on the separation of selected alkaloids on CN-silica layers
ABSTRACTSelected alkaloids were chromatographed on cyanopropyl-silica thin layers using nonaqueous and aqueous eluents containing various free silanol blocker agents. Because of the strong retention of these basic compounds, nonaqueous eluents containing medium polar diluents, strongly polar modifiers, or aqueous eluents containing organic modifier, water, and silanol blockers (ammonia, diethylamine, and ionic liquid) were required for analysis. Mobile phases containing addition of acids were also tested for separation of investigated alkaloids. The most selective and efficient systems were used in two-dimensional separations of isoquinoline alkaloids’ mixture and plant extracts. 相似文献