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101.
De-en Han Yanmei Shi Ping Tian Hengchao Wei Mingsan Miao Xiu-min Li 《Biomedical chromatography : BMC》2020,34(7):e4838
A rapid and sensitive method was developed and validated for the quantitative determination of xanthopurpurin (XPP) in rat plasma using ultra-performance liquid chromatography-electrospray ionization-Orbitrap mass spectrometry. XPP inhibits IgE production and prevents peanut-induced anaphylaxis. The XPP and emodin (internal standard) were determined in negative ion mode with m/z 239.0350 → 211.0400 and 269.0455 → 241.0507, respectively. The separation process was achieved using an ACQUITY UPLC HSS T3 column with acetonitrile and 0.1% formic acid in water (85:15). The linear range was 0.5–100 ng/mL, and the correlation coefficient (r2) was > 0.993. The inter-day and intra-day precision was within an acceptable range of 15%. The extraction recovery and matrix effect were 78.9–87.2% and 94.3–98.5%, respectively. Under different conditions, the XPP was stable in the range of 5.6–10.6%. This method was successfully applied to study the pharmacokinetics of XPP with an oral dose of 10.0 mg/kg and intravenous dose of 2.0 mg/kg in rats. The absolute oral bioavailability of XPP was 4.6%. 相似文献
102.
Jihua Liu Huizhu Gan Ting Li Jia Wang Guangguang Du Yang An Xiaojing Yan Cong Geng 《Biomedical chromatography : BMC》2020,34(8):e4856
Ocotillol, pseudo-ginsenoside RT5 (RT5), and pseudo-ginsenoside F11 (PF11) are ocotillol-type saponins that have the same aglycone structure but with different numbers of glucose at the C-6 position. In this study, the metabolites of ocotillol, RT5, and PF11 in rat plasma, stomach, intestine, urine, and feces after oral administration were investigated by ultra-performance liquid chromatography coupled with time-of-flight mass spectrometry. The results showed that RT5 was easily biotransformed into metabolites in vivo, whereas PF11 and RT5 were difficult to be biotransformed. Hydrogenation, dehydrogenation, dehydration, deglycosylation, deoxygenation, hydration, phosphorylation, deoxidation, glucuronidation, and reactions combining amino acid were speculated to be involved in the biotransformation of ocotillol, RT5, and PF11. Based on the structural analysis of metabolites, it was deduced that hydrogenation, dehydration, deoxidation, and reactions combining amino acid occurred on the aglycone structure, whereas deglycosylation, hydration, and phosphorylation occurred on the glycosyl chain. Further, metabolites in plasma, urine, feces, and tissues were different: First, glucuronidation products were found in urine, stomach, intestine, and feces, but not in plasma. Second, the ocotillol prototype was not identified in urine samples. Third, the RT5 prototype was found in stomach, intestine, feces, and urine, but not in plasma. 相似文献
103.
Jia Yang Xingang Li Wenjun Li Xin Xi Qian Du Feng Pan Songqing Liu 《Biomedical chromatography : BMC》2020,34(8):e4857
Because of its unpredictable side effects and efficacy, the anticancer drug docetaxel (DTX) requires improved characterisation of its pharmacokinetic profiles through population pharmacokinetic studies. A sensitive and rugged LC–MS/MS method for the detection of DTX in human plasma was developed and optimised using paclitaxel as an internal standard (IS). The plasma samples underwent rapid extraction using hybrid solid-phase extraction-protein precipitation. The analyte and IS were separated with an isocratic system on a Zorbax Eclipse Plus C18 column using water containing 0.05% acetic acid along with 20 μM of sodium acetate and methanol (30/70, v/v) as the mobile phase. Quantification was performed using a triple quadrupole mass spectrometer through multiple reaction monitoring in positive mode, using the m/z 830.3 → 548.8 and m/z 876.3 → 307.7 transitions for DTX and paclitaxel, respectively. The range of the calibration curve was 1–500 ng/mL for DTX, and the linear correlation coefficient was >0.99. The accuracies ranged from −4.6 to 4.2%, and the precision was no higher than 7.0% for the analytes. No significant matrix effect was observed. Both DTX and the IS showed considerable recovery. This method was finally applied to the establishment of a population pharmacokinetic model to optimise the clinical use of DTX. 相似文献
104.
Ziritaxestat is a first-in-class autotoxin inhibitor. The purpose of this study was to develop a liquid chromatography/electrospray ionization tandem mass spectrometric (LC–MS/MS) method for the determination of ziritaxestat in rat plasma. The plasma sample was deproteinated using acetonitrile and then separated on an Acquity BEH C18 column with water containing 0.1% formic acid and acetonitrile as mobile phase, which was delivered at 0.4 ml/min. Ziritaxestat and the internal standard (crizotinib) were quantitatively monitored with precursor-to-product transitions of m/z 589.3 > 262.2 and m/z 450.1 > 260.2, respectively. The total running time was 2.5 min. The method showed excellent linearity over the concentration range 0.5–2000 ng/ml, with correlation coefficient >0.9987. The extraction recovery was >82.09% and the matrix effect was not significant. Inter- and intra-day precisions (RSD) were <11.20% and accuracies were in the range of −8.50–7.45%. Ziritaxestat was demonstrated to be stable in rat plasma under the tested conditions. The validated LC–MS/MS method was successfully applied to study the pharmacokinetic profiles of ziritaxestat in rat plasma after intravenous and oral administration. Pharmacokinetic results demonstrated that ziritaxestat displayed a short half-life (~3 h) and low bioavailability (20.52%). 相似文献
105.
Yining Liu Canhui Chen Jiuwen Qiu Zongbao Fang Haibo Wu Xingxian Zhang Shufang Wang 《Biomedical chromatography : BMC》2019,33(3)
Hongjingtian injection is made from Rhodiola wallichiana and used in the treatment of stable angina pectoris associated with coronary heart disease. In this study, the chemical constituents in Hongjingtian injection were comprehensively studied using liquid chromatography quadrupole time‐of‐flight mass spectrometry. A total of 49 compounds were identified or assumed, including 10 organic acids, nine phenylethanoids, 10 phenylpropanoids, two flavonoid glycosides, seven monoterpene glycosides, seven octylglycosides and four other types of compounds. The structures of seven compounds were confirmed by comparing their retention times, MS and UV spectra with the corresponding authentic standards. Amongst the 49 compounds, 35 were firstly found in R. wallichiana, while they have been reported in other species of the genus Rhodiola, including Rhodiola crenulata, Rhodiola sacra, Rhodiola rosea and Rhodiola kirilowii. The possible fragmentation pathways in the mass spectrometry of the major types of compounds are proposed and summarized. Our study demonstrates a rapid method for characterizing the chemical constituents present in the Hongjingtian injection, which could also be applied to the identification of chemical constituents in other TCM formulae containing R. wallichiana. 相似文献
106.
Jie Wang Cuicui Ma Qiannan Li Xing Wang Yang Yang Lingjian Yang Wei Jiang Sha Liao Shixiang Wang Pu Jia Ye Zhao Xiaohui Zheng 《Biomedical chromatography : BMC》2019,33(3)
Tanshinol borneol ester (DBZ) is a potential drug candidate composed of danshensu and borneol. It shows anti‐ischemic and anti‐atherosclerosis activity. However, little is known about its metabolism in vivo. This research aimed to elucidate the metabolic profile of DBZ through analyzing its metabolites using high‐performance liquid chromatography combined with electrospray ionization quadrupole time‐of‐flight mass spectrometry. Chromatographic separation was performed on an Agilent TC‐C18 column (150 × 4.6 mm, 5.0 μm) with gradient elution using methanol and water containing 0.2% (v/v) formic acid as the mobile phase. Metabolite identification involved analyzing the retention behaviors, changes in molecular weights and MS/MS fragment patterns of DBZ and its metabolites. As a result, 20 potential metabolites were detected and tentatively identified in rat plasma, urine and feces after administration of DBZ. DBZ could be metabolized to O‐methylated DBZ, DBZ‐O‐glucuronide, O‐methylated DBZ‐O‐glucuronide, hydroxylated DBZ and danshensu. Danshensu, a hydrolysis product of DBZ, could further be transformed into 12 metabolites. The proposed method was confirmed to be a reliable and sensitive alternative for characterizing metabolic pathways of DBZ and providing valuable information on its druggability. 相似文献
107.
Lin Hui-Min Mu Chao Li Ao Liu Xu-Feng Li Yu-Long Jiang Zhong-Qing Wu Hong-Ke 《Transition Metal Chemistry》2019,44(5):491-498
Transition Metal Chemistry - In this paper, four diiron toluene-3,4-dithiolate complexes with phosphine ligands were synthesized and characterized. Treatment of complex... 相似文献
108.
Qiao Wang Lefan Li Zongjin Li Siyao Guo Guoxing Sun 《Journal of Polymer Science.Polymer Physics》2019,57(11):713-721
It remains challenging to satisfy the combined performances for hydrogels with excellent mechanical behavior, high deformability, and super recoverability under harsh environmental conditions. In this study, we first established a strong polymer network via the crosslinking of polymer chains on the surfaces of sub‐5‐nm calcium hydroxide nanospherulites in ethylene glycol solvent. The organic gel expressed excellent mechanical properties such as a recoverable compressive engineering stress of 249 MPa and an elongation stress of 402 KPa, which was attributed to the uniform nanosized crosslinking structure as characterized by SEM. Moreover, the nonvolatile solvent remained in the gel, meaning that the sample can resist a wide temperature range of ?56 to 100 °C without losing the elastic properties. This novel organic gel could provide promising routes to develop the ideal elastic carriers for wearable devices, smart skin sensors, and damping materials. © 2019 Wiley Periodicals, Inc. J. Polym. Sci., Part B: Polym. Phys. 2019 , 57, 713–721 相似文献
109.
Let be a connected graph with edges. An antimagic labeling of is a one-to-one mapping from to such that the vertex sum (i.e., sum of the labels assigned to edges incident to a vertex) for distinct vertices are different. A graph is called antimagic if has an antimagic labeling. It was conjectured by Hartsfield and Ringel that every tree other than is antimagic. The conjecture remains open though it was verified for trees with some constrains. Caterpillars are an important subclass of trees. This paper shows caterpillars with maximum degree 3 are antimagic, which gives an affirmative answer to an open problem of Lozano et al. (2019). 相似文献
110.
Torin F. Stetina Aurora E. Clark Xiaosong Li 《International journal of quantum chemistry》2019,119(1):e25802
Despite fundamental importance, the experimental characterization of the hydrogen bond network, particularly in multicomponent protic solutions, remains a challenge. Although recent work has experimentally validated that the oxygen K-edge X-ray absorption spectra is sensitive to local hydrogen bond patterns in pure water and aqueous alcohol solutions, the generality of this observation is unknown—as is the sensitivity to the electronic structure of the alcohol cosolvent. In this work, we investigate the electronic structure of water solvated alcohol model geometries using energy specific time-dependent density functional theory to calculate oxygen K-edge X-ray excitations. We find that the geometry of dangling hydrogen bonds in pure water is the main contributor to the pre-edge feature seen in the X-ray absorption spectra, agreeing with previous experimental and theoretical work. We then extend this result to solvated alcohol systems and observe a similar phenomenon, yet importantly, the increase of electron donation from alkyl chains to the alcohol OH group directly correlates to the strength of the core excitation on the dangling hydrogen bond model geometry. This trend arises from a stronger transition dipole moment due to electron localization on the OH group. 相似文献