ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2022
·Vol. 415
·期 3
·493-507
·
IF 4.478
Li Zhuoya,Huang Xinyi,Wang Xuan,Ren Jianwei,Xu Buyi,Luo Chunying,Wang Yanjun,Wang Lian,Harada Kouji H.,Zou Xiaoli
A rapid and sensitive high-performance liquid chromatography–high-resolution orbitrap mass spectrometry method was developed for the simultaneous screening of 354 organic poisons and metabolites in blood and urine, including drugs, medications, pesticides, rodenticides, veterinary drugs, alkaloids, and mycotoxins with a multi-toxicant chromatography-mass spectrometry information library. The method and library showed good prospects in clinical poisoning screening and forensic toxicological identification. Blood and urine samples were extracted successively with ethyl acetate in acidic and alkaline conditions; then, the extract was blown to nearly dry by nitrogen gas and redissolved with methanol-aqueous solution (v:v, 50:50), and the dissolved solution was analyzed by LC-MS/MS after filtering. Precursor ions’ m / z was set for identification, retention time, fragment ions, and isotopic pattern which were used for confirmation. No interference peaks were found in the blank samples, showing good specificity. The LODs of toxicants in urine and blood were 1.00×10 −3 –50.0 ng/mL and 2.07×10 −3 –50.0 ng/mL, respectively, while the LOQs were 3.30×10 −3 –1.67×10 2 ng/mL and 6.91×10 −3 –1.67×10 2 ng/mL. The intra-day precision and inter-day precision of urine samples were 2.31–9.13% and 4.75–12.3%, respectively, which were 1.92–10.8% and 2.01–12.1% in blood samples. The established method was applied to analyze 9 cases of clinical poisoning patients, and bromadiolone, carbofuran, and amanitins were detected, respectively. A total of 382 biospecimens from drug abusers were analyzed with the proposed method, which indicated that some drugs were detected in 62 cases, mainly including methamphetamine, heroin, and MDMA. The results were consistent with the information from traditional liquid chromatography-triple quadrupole mass spectrometry. Graphical abstract
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PubMed
高影响因子
CHROMATOGRAPHIA
·
2018
·Vol. 81
·期 9
·1257-1267
·
IF 1.401
Guo Wei,Li Ben,Chi Haijun,Ramsey Edward D.
Abstract The operation of a SFC–MS system has been improved. The SFC–MS interface uses a post-column make-up flow of liquid whose supply line to the SFC–MS interface mixing tee is equipped with an injection valve. Prior to analysis, this arrangement permits a stable flow of a dilute tune solution of analyte(s) for the exact amount of time required to optimize mass spectrometry tuning. Advantageously, with this arrangement tuning is performed in the presence of the exact split flow and same composition of SFC mobile phase and make-up liquid to be used for subsequent SFC–MS operation. The SFC–MS interface was constructed to provide a pre-back pressure regulator split flow to the mass spectrometer using a linear restrictor. Two different linear restrictors constructed from either 50 µm i.d. PEEK tubing or 25 µm i.d. fused silica tubing were evaluated. For best electrospray performance, each restrictor required a different post-column make-up flow rate. The use of either restrictor retained a high degree of chromatographic fidelity for the SFC separation of six pharmaceutical compounds using a cyanopropyl column with a mobile phase of supercritical fluid carbon dioxide modified with methanol and aqueous ammonia solution. Each restrictor provided a different level of SFC–MS performance for each of the six pharmaceutical compounds tested. Based upon overall performance, a linear fused silica restrictor was selected to develop a chromatographic separation using on-line SFC–MS for three structurally very similar monensin sodium salt analogues that are not directly amenable to off-line SFC using UV/Vis detection. Graphical abstract
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高影响因子
Scientific Reports
·
2017
·Vol. 7
·期 1
·1-10
·
IF 4.259
Wang Guojing,Jing Shengchang,Tan Yiwei
Shape control of noble metal (NM) nanocrystals (NCs) is of great importance for improving their electrocatalytic performance. In this report, branched Pd@Rh core@shell NCs that have right square prism-like arms with preferential exposure of Rh {100} facets (denoted as b-Pd@Rh-NCs thereafter) are synthesized and utilized as an electrocatalyst for the hydrazine electrooxidation (HEO) in acidic and alkaline electrolytes. The b-Pd@Rh-NCs are obtained by the heteroepitaxial growth of Rh on the pre-formed branched Pd NCs (denoted as b-Pd-NCs thereafter) core in the presence of poly(vinyl pyrrolidone) (PVP) and bromide ions. A comparative analysis of the voltammetric data for the HEO shows a higher activity on the b-Pd@Rh-NCs exposed with Rh {100} faces than on Rh black, the b-Pd-NCs, and Pd black in acid and alkaline solutions, indicating a structure sensitivity of the reaction. Analysis of the products from the b-Pd@Rh-NCs catalysed HEO reveals a very high hydrazine fuel efficiency, as determined by on-line differential electrochemical mass spectrometry (DEMS).
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DOI
PubMed
高影响因子
GLYCOCONJUGATE JOURNAL
·
2018
·Vol. 35
·期 4
·411-420
·
IF 2.548
Wang Chengjian,Yang Meifang,Gao Xi,Li Cheng,Zou Zihua,Han Jianli,Huang Linjuan,Wang Zhongfu
Despite the great significance of release and analysis of glycans from glycoproteins, the existing N -glycan release methods are undermined by some limitations and deficiencies. The traditional enzymatic protocols feature high N -glycan release specificity but are generally costly and inefficient for some types of N -glycans. The existing chemical methods require harsh reaction conditions or are accompanied by the remarkable formation of by-products. Herein, we describe a versatile chemical method for the release and analysis of N -glycans from glycoproteins. This method differs from the existing methods as only aqueous ammonia is used to catalyze the N -glycan release reactions. Optimization of reaction conditions was performed using RNase B as a model glycoprotein and the obtained results indicated a highest N -glycan yield in ammonia at 60 °C for 16 h. Comparison of this method with traditional enzymatic protocols and recently reported NaClO methods confirmed the good reliability and efficiency of the novel approach. We also successfully applied this method to some complex biological samples, such as Ginkgo seed protein, fetal bovine serum (FBS) and hen egg white, and demonstrated its great compatibility with various neutral N -glycans, core α-1,3-fucosylated N -glycans and sialylated N -glycans. This method is very simple and cost-effective, enabling convenient analysis and large-scale preparation of released reducing N- glycans from various biological samples for structural and functional glycomics studies.
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DOI
PubMed
高影响因子
JOURNAL OF RADIOANALYTICAL AND NUCLEAR CHEMISTRY
·
2020
·Vol. 325
·期 2
·673-682
·
IF 1.137
Liu Bing,Jia Yongzhong,Jing Yan,Zhang Quanyou,Shao Fei,Yao Ying
Abstract The lithium isotope separation (LIS) plays a vital role in development of nuclear industry. The liquid–liquid extraction technologies open up new possibilities for LIS. This work presents preliminary results of the study on the extractions and separation of 6 Li/ 7 Li by mixed system, comprising amino-derivatives of benzo-15-crown-5 (4AB), ionic liquid and anisole. 4AB was used as an extractant. The eparation factor ( α ) is 1.031 ± 0.001, and abundance of 6 Li in loaded organic phase is 7.76%. Meanwhile, the reason why 4AB has better separation efficiency than B15C5 was explored brief by Fourier transform infrared (FT-IR) spectrum and quantum chemical calculations. Graphic abstract
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高影响因子
JOURNAL OF NANOPARTICLE RESEARCH
·
2019
·Vol. 21
·期 7
·1-16
·
IF 2.009
Li Guiyin,Zeng Junxiang,Zhao Le,Wang Zhihong,Dong Chenyang,Liang Jintao,Zhou Zhide,Huang Yong
Cholesterol is a waxy steroid metabolite substance and plays an important role in the brain, nervous, and immune systems of humans. The level of cholesterol in human serum has become an important index for clinical diagnosis and prevention of cardiovascular disease. In this study, a highly sensitive electrochemical biosensor for cholesterol measurement has been developed based on reduced graphene oxide-chitosan-ferrocene carboxylic acid/platinum nanoparticle (RGO-CS-Fc/Pt NPs) modified screen-printed carbon electrode (SPCE). Under the effect of cholesterol oxidase (CHOD) and cholesterol esterase (CHER), the cholesterol was oxidized to generate hydrogen peroxide (H 2 O 2 ), which can be disintegrated into H 2 O with the synergistic catalysis of RGO-CS-Fc/Pt NPs and produce the redox response current of H 2 O 2 that could be determined by electrochemical amperometric (i-t) method. The prepared cholesterol biosensor was achieved by integrating of the high electrocatalytic efficiency of Pt NPs, high electronic conductivity and large surface area of RGO, the reversible electrochemical behavior of Fc, and good biocompatibility of CS. The measured of redox response current and cholesterol concentration have a good linearity in the range of 0.5–4.0 mg/mL, low detection limit of 5.70 μg/mL (S/N = 3), and good sensitivity of 0.871 nA/mM/cm 2 . Moreover, the RGO-CS-Fc/Pt NPs cholesterol biosensor exhibited excellent specificity, acceptable reproducibility, and higher recoveries in the detection of clinical serum samples, showing great potential for clinical diagnosis.
Schematic presentation of an electrochemical biosensor based on RGO-CS-Fc/Pt NPs for cholesterol detection.
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高影响因子
CATALYSIS LETTERS
·
2017
·Vol. 147
·期 10
·2534-2541
·
IF 2.799
Zhang Chenjun,Lu Dan,Jiang Pingping,Li Jingjing,Leng Yan
Abstract A novel porous cross-linked chitosan polymer was prepared by Schiff reaction of chitosan (CS) with terephthalic aldehyde (TPA), followed by modification with trimethoxysilylpropanethiol. Such functional CS polymer (CS-TPA) could serve as both support and stabilizer for homogeneous palladium (Pd 2+ ) catalyst. The obtained heterogeneous catalyst (Pd/CS-TPA-SH) exhibited high catalytic activity and selectivity for the oxidative Heck reaction of benzene and ethyl acrylate. The excellent performance is mostly attributed to the –SH groups stabilized Pd 2+ species. Furthermore, Pd/CS-TPA-SH can also be used as the catalyst for the reduction of p-nitrophenol at room temperature, showing high efficiency and steady reusability. Graphical Abstract A novel thiol functionalized cross-linked chitosan polymer supporting palladium is synthesized and proved to be a highly efficient catalyst for oxidative Heck reaction and nitrophenol reduction.
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高影响因子
Frontiers of Environmental Science & Engineering
·
2012
·Vol. 6
·期 4
·445-454
·
IF 0
Li Wenzhen,Ding Yu,Sui Qian,Lu Shuguang,Qiu Zhaofu,Lin Kuangfei
The aim of this study was to identify the intermediates in clofibric acid degradation under various advanced oxidation processes, namely ultraviolet (UV), UV/H 2 O 2 , vacuum ultraviolet (VUV), VUV/H 2 O 2 , and solar/TiO 2 processes, as well as to assess the toxicity of these intermediates. Eleven intermediates have been detected by gas chromatography-mass spectrometer, most of which were reported for the first time to our best knowledge. Combining the evolution of the dissolved organic carbon, Cl − and specific ultraviolet absorption at 254 nm, it could be deduced that cleavage of aromatic ring followed by dechlorination was the mechanism in solar/TiO 2 process, while dechlorination happened first and accumulation of aromatic intermediates occurred in the other processes. Different transformation pathways were proposed for UV-, VUV-assisted and solar/TiO 2 processes, respectively. The acute toxicity was evaluated by means of Photobacterium phosphoreum T 3 spp. bioassay. It was believed that aromatic intermediates increased the toxicity and the ring-opening pathway in solar/TiO 2 process could relieve the toxicity.
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DOI
Frontiers of Materials Science
·
2015
·Vol. 9
·期 4
·366-372
·
IF 1
Xia Yu,Ma Liang,Lu Hui,Wang Xian-Ping,Gao Yun-Xia,Liu Wang,Zhuang Zong,Guo Li-Jun,Fang Qian-Feng
Garnet-like Li 6.8 La 3 Zr 1.8 Bi 0.2 O 12 (LLZBO) + x mol.% Al 2 O 3 ( x = 0, 1.25, 2.50) lithium ionic electrolytes were prepared by conventional solid state reaction method under two different sintering temperatures of 1000°C and 1100°C. XPS, induced coupled plasma optical emission spectrometer (ICP-OES), XRD and AC impedance spectroscopy were applied to investigate the bismuth valance, lithium concentration, phase structure and lithium ionic conductivity, respectively. Electrical measurement demonstrated that ionic conductivity of Al-added LLZBO compounds could be obviously improved when the sample sintering temperature increased from 1000°C to 1100°C. The highest ionic conductivity 6.3×10 -5 S/cm was obtained in the LLZBO-1.25%Al sample sintered at 1100°C, in consistent with the lowest activation energy 0.45 eV for the lithium ion migration. The mechanism related with good ionic conductivity in the Al-added LLZBO sample was attributed to the lattice distortion induced by the partial Al substitution at Zr sites, which is helpful to improve the migration ability of Li ions in lattice.
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高影响因子
Frontiers of Chemical Science and Engineering
·
2021
·Vol. 16
·期 4
·484-497
·
IF 4.204
Yang Jinian,Feng Xuesong,Nie Shibin,Xu Yuxuan,Li Zhenyu
The nanocomposites of flower-like nickel phyllosilicate particles incorporated into epoxy resin were fabricated via an in-situ mixing process. The flower-like nickel phyllosilicate particles were firstly synthesized using a mild self-sacrificial templating method, and the morphology and lamellar structure were examined carefully. Several properties of mechanical, thermal and tribological responses of epoxy nanocomposites were performed. It was demonstrated that adequate flower-like nickel phyllosilicate particles dispersed well in the matrix, and the nanocomposites displayed enhanced tensile strength and elastic modulus but decreased elongation at break as expected. In addition, friction coefficient and wear rate were increased first and then decreased along with the particle content, and showed the lowest values at a mass fraction of 5%. Nevertheless, the incorporated flower-like nickel phyllosilicate particles resulted in the continuously increasing thermal stability of epoxy resin (EP) nanocomposites. This study revealed the giant potential of flower-like particles in preparing high-quality EP nanocomposites.
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高影响因子
Frontiers of Physics
·
2023
·Vol. 18
·期 3
·1-12
·
IF 7.5
Liao Qiugang,Liu Hao,Chen Ziqiang,Zhang Yinggan,Xiong Rui,Cui Zhou,Wen Cuilian,Sa Baisheng
With the development of modern electronics, especially the next generation of wearable electromagnetic interference (EMI) shielding materials requires flexibility, ultrathin, lightweight and robustness to protect electronic devices from radiation pollution. In this work, the flexible and ultrathin dopamine modified MXene@cellulose nanofiber (DM@CNF) composite films with alternate multilayer structure have been developed by a facile vacuum filtration induced self-assembly approach. The multilayered DM@CNF composite films exhibit improved mechanical properties compared with the homogeneous DM/CNF film. By adjusting the layer number, the multilayered DM3@CNF2 composite film exhibits a tensile strength of 48.14 MPa and a toughness of 5.28 MJ·m − 3 with a thickness about 19 µm. Interestingly that, the DM@CNF film with annealing treatment achieves significant improvement in conductivity (up to 17264 S·m −1 ) and EMI properties ( SE of 41.90 dB and SSE/t of 10169 dB·cm 2 ·g − 1 ), which still maintains relatively high mechanical properties. It is highlighted that the ultrathin multilayered DM@CNF film exhibits superior EMI shielding performance compared with most of the metal-based, carbon-based and MXene-based shielding materials reported in the literature. These results will offer an appealing strategy to develop the ultrathin and flexible MXene-based materials with excellent EMI shielding performance for the next generation intelligent protection devices.
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高影响因子
Frontiers of Environmental Science & Engineering
·
2015
·Vol. 10
·期 3
·438-446
·
IF 1.357
Xu Minhui,Gu Xiaogang,Lu Shuguang,Miao Zhouwei,Zang Xueke,Wu Xiaoliang,Qiu Zhaofu,Sui Qian
The thermally activated persulfate (PS) degradation of carbon tetrachloride (CT) in the presence of formic acid (FA) was investigated. The results indicated that CT degradation followed a zero order kinetic model, and CO
– 2
· was responsible for the degradation of CT confirmed by radical scavenger tests. CT degradation rate increased with increasing PS or FA dosage, and the initial CT had no effect on CT degradation rate. However, the initial solution pH had effect on the degradation of CT, and the best CT degradation occurred at initial pH 6. Cl – had a negative effect on CT degradation, and high concentration of Cl – displayed much strong inhibition. Ten mmol·L –1 HCO
– 3
promoted CT degradation, while 100 mmol·L – 1NO
– 3
inhibited the degradation of CT, but SO
2– 4
promoted CT degradation in the presence of FA. The measured Cl–concentration released into solution along with CT degradation was 75.8% of the total theoretical dechlorination yield, but no chlorinated intermediates were detected. The split of C-Cl was proposed as the possible reaction pathways in CT degradation. In conclusion, this study strongly demonstrated that the thermally activated PS system in the presence of FA is a promising technique in in situ chemical oxidation (ISCO) remediation for CT contaminated site.
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高影响因子
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