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Ultra‐performance liquid chromatography coupled with electrospray ionization/quadrupole time‐of‐flight mass spectrometry for the rapid analysis of constituents in the traditional Chinese medical formula Danggui San 下载免费PDF全文
In this work, ultra‐performance LC with ESI quadrupole TOF‐MS (UPLC–ESI‐Q‐TOF‐MS) and automated MetaboLynx analysis was used to rapidly separate and identify the chemical constituents of Danggui San, a traditional Chinese medical formula. The analysis was performed on a Waters UPLC BEH C18 column using a gradient elution system. A hyphenated ESI and Q‐TOF analyzer was used for the determination of the accurate mass of the protonated or deprotonated molecule and fragment ions in both positive and negative modes. Based on retention times, accurate mass, and the mass spectrometric fragmentation characteristics, a total of 47 compounds distributed over the chemical groups of phthalides, flavonoids, monoterpene glycosides, sesquiterpenoids, phenolics, and alkaloids, were simultaneously separated within 18 min and identified or tentatively elucidated in Danggui San for the first time. UPLC–ESI‐Q‐TOF‐MS analysis revealed the complexity of the chemical composition of this formula. The method developed is rapid, accurate, reliable, and highly sensitive to characterize the chemical constituents of Danggui San. 相似文献
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Chunxiao Lv Qing Li Yaowen Zhang Zhenyu Sui Bosai He Huarong Xu Yidi Yin Xiaohui Chen Kaishun Bi 《Journal of mass spectrometry : JMS》2013,48(8):904-913
A fast, sensitive and reliable ultra fast liquid chromatography‐tandem mass spectrometry (UFLC‐MS/MS) method has been developed and validated for simultaneous quantitation of polygalaxanthone III (POL), ginsenoside Rb1 (GRb1), ginsenoside Rd (GRd), ginsenoside Re (GRe), ginsenoside Rg1 (GRg1) and tumulosic acid (TUM) in rat plasma after oral administration of Kai‐Xin‐San, which plays an important role for the treatment of Alzheimer's disease (AD). The plasma samples were extracted by liquid–liquid extraction using ethyl acetate–isopropanol (1:1, v/v) with salidrdoside as internal standard (IS). Good chromatographic separation was achieved using gradient elution with the mobile phase consisting of methanol and 0.01% acetic acid in water. The tandem mass spectrometric detection was performed in multiple reaction monitoring mode on 4000Q UFLC‐MS/MS system with turbo ion spray source in a negative and positive switching ionization mode. The lower limits of quantification were 0.2–1.5 ng/ml for all the analytes. Both intra‐day and inter‐day precision and accuracy of analytes were well within acceptance criteria (±15%). The mean absolute extraction recoveries of analytes and IS from rat plasma were all more than 60.0%. The validated method has been successfully applied to comparing pharmacokinetic profiles of analytes in normal and AD rat plasma. The results indicated that no significant differences in pharmacokinetic parameters of GRe, GRg1 and TUM were observed between the two groups, while the absorption of POL and GRd in AD group were significantly higher than those in normal group; moreover, the GRb1 absorbed more rapidly in model group. The different characters of pharmacokinetics might be caused by pharmacological effects of the analytes. Copyright © 2013 John Wiley & Sons, Ltd. 相似文献
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蒙药三子散由诃子、川楝子、栀子3味药材等比例组成,其临床用药主要采用口服给药方式,药物在体内的吸收、分布、代谢、排泄过程与药物发挥药理作用和疗效的产生密切相关,因此考察灌胃给药后的入血成分有助于阐明三子散的药效物质基础。研究采用血清药物化学研究思路,将Wistar大鼠分成空白组和给药组,给药组给予三子散水提物,腹主动脉取血,离心制备血清样品,采用高效液相色谱-四极杆/静电场轨道阱高分辨质谱(HPLC-Q/Orbitrap HRMS),在SHIMADZU GIST C18色谱柱(150 mm×4.6 mm, 5 μm)上进行色谱分离;以甲醇和0.1%(v/v)甲酸水溶液为流动相进行梯度洗脱,柱温30 ℃,流速0.5 mL/min,进样量10 μL,采用加热电喷雾电离(HESI)源,正、负离子同时扫描。通过比对三子散含药血清和空白血清的图谱差异,查阅数据库、各类成分体内代谢途径、三子散成分的相关文献,采用Xcalibur 3.0软件进行峰提取、峰匹配等质谱数据处理,结合Compound Discover 3.0软件对化合物代谢途径的预测分析和裂解规律的推断,解析三子散水提液经大鼠灌胃后血清中的原型成分和代谢产物。结果表明,在给药大鼠血清样品中鉴定出55种入血成分,其中41种原型成分,14种代谢产物。入血的原型成分主要为鞣质类、环烯醚萜类和小分子酚酸类。该研究较为全面地阐释了三子散水提液在大鼠血中的移行成分,有助于揭示三子散的药效物质基础,为该药的临床应用提供参考。 相似文献
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Kathryn M. Kuivila Bryan E. Jennings 《International journal of environmental analytical chemistry》2013,93(13-14):897-911
Temporal patterns of pesticide inputs to San Francisco Bay were identified and correlated with timing of application and transport mechanism. Fluxes were calculated from measured concentrations and estimated flow. Persistence of the pesticides under typical riverine or estuarine conditions were estimated from laboratory experiments. Simazine was detected most frequently and had the highest flux into the Bay, which could be explained by its continuous use and long half-life. In comparison, diazinon was detected at lower concentrations and had a lower flux which corresponded to its lower use and shorter half-life. The order-of-magnitude lower fluxes of carbofuran and methidathion corresponded to their lower use and expected hydrolysis. Molinate was detected at the highest concentration but its flux was lower than expected, considering its very high use and persistence in the laboratory experiments. Additional loss of molinate is likely to occur from volatilization and photodegradation on the rice fields. Although thiobencarb had the second highest use, it had the lowest flux of the six pesticides, which can be attributed to its loss via hydrolysis, photodegradation, volatilization, and sorption to sediments. Fluxes into San Francisco Bay were equal to or greater than those reported for other estuaries, except for the Gulf of Mexico. 相似文献
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梨圆蚧是对果林危害较大的害虫。该虫的性信息素包括三个组分:3-亚甲基-7-甲基-7-辛烯-1-醇丙酸酯(1)、(2Z)-3,7-二甲基-2,7-辛二烯-1-醇丙酸酯(2)和(2E)-3,7-二甲基-2,7-辛二烯-1-醇丙酸酯(3)。本文介绍了通过对月桂烯进行结构改造来合成梨圆蚧性信息素,从月桂烯到1,总产率为19%。工业上从月桂烯制龋萑花醇和香叶醇,再将橙花醇和香叶醇转变为相应的氯烯醇后再还原、丙酰化即得2和3,其总产率分别为30%和28%。(以橙花醇和香叶醇计)。月桂烯可从β-蒎烯裂解而得。我国有丰富的蒎烯资源,所以开辟从月桂烯合成梨圆蚧性信息素的新途径具有重要的意义。 相似文献
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The Nesbet cluster expansion for atoms and molecules is extended to much more general situations than previously assumed possible. To exemplify non-conventional uses of the equation the one-dimensional half-filled Hubbard model is evaluated; results are in good agreement with the known exact solution. A possible way of applying the same procedure to realistic hamiltonians is discussed. 相似文献
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Gas phase electron diffraction data for HFDB were analyzed, following conventional procedures, and a structure was deduced for the perfluoro-bicyclo-[2.2.0]hexa-2,5-diene consistent with its C2v symmetry. A least squares analysis of the molecular scattering function gave the following rg values: [-C-C-] = 1.597 ± 0.006 Å, [C-C-] = 1.503 ± 0.002 Å, [-C-C-] = 1.356 ± 0.007 Å, [-C-F](bridge) = 1.331 ± 0.008 Å, [-C-F] (terminal) = 1.323 ± 0.004 Å. The flap angle between the rings is 115.3( ± .7)°. The terminal fluorines are in the planes of the corresponding rings.The most notable feature of the structure is the long C-C bridge bond, which was also observed in hexamethyl-Dewar-benzene. The geometrical features of HFDB are compared with corresponding ones in HMDB, and with perfluoro- cyclobutene as well as with theoretical estimates. 相似文献
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电感耦合等离子体原子发射光谱测定生脉散中多种微量元素 总被引:4,自引:0,他引:4
采用ICP-AES法测定生脉散中多种微量元素,考查不同品种人参的煎煮液中多种微量元素的溶出情况。实验表明人参、麦冬、五味子生药材及水煎液经硝酸-高氯酸体系消化,样品消解完全,可以满足ICP-AES检测的要求。结果的相对标准偏差为0.70%~5.9%,加标回收率为95.2%~112.4%,各种微量元素的溶出率以西洋参、麦冬、五味子为复方药的共煎液中溶出率较高,从而进一步证实了生脉散该复方药的合理性。文章为药剂学研究提出了一个简便、准确和可行的研究方法的同时,也对中药复方的合理性进行了考察,为其临床疗效研究提供了有效依据。 相似文献
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Tianxue Li Zhixiang Yan Chen Zhou Jian Sun Chuan Jiang Xinghao Yang 《Biomedical chromatography : BMC》2013,27(8):1041-1053