ANALYTICAL SCIENCES
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2021
·Vol. 37
·期 10
·1413-1418
·
IF 2.081
Hua ZHAO,Xiaohui WANG,Yuli ZHANG,Xiaowan HUANG,Yaling JIANG,Huan MA,Li AN,Xujin WU,Qiang WANG
Saikosaponin a and saikosaponin d are used as chemical standards for the quality evaluation of Bupleurum chinense DC. by the high-performance liquid chromatography method in current Chinese Pharmacopoeia. However, other saikosaponins, such as saikosaponin c and saikosaponin b2, also possess pharmaceutical activity, but are not used as chemical standards. In this study, a quantitative proton nuclear magnetic resonance (1H NMR) method was developed to determine the total mass percentage (mg/g) of SSa, SSb1, SSb2 and SSd in B. chinense DC., using the H-24 (δH 0.71) signal. Furthermore, the molality (mol/kg) of type I saikosaponins (epoxy-ether structure) was also determined by quantitative 1H NMR in the area of H-11 (δH 5.95) for a more accurate quality evaluation. Validation of the method confirmed that it has acceptable selectivity, precision, stability, and repeatability. The results indicated that this method has the potential to be a reliable method for the quantification of saikosaponins in Bupleurum scorzonerifolium Willd., vinegar baked B. chinense DC. and B. scorzonerifolium Willd., Chaihu Koufuye (oral liquid of Chaihu).
研究领域:
药学化学
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分析化学
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生药学
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DOI
PubMed
高影响因子
Analytical Methods
·
2019
·Vol. 11
·期 48
·6176-6183
·
IF 2.378
Fei-Fei Li,Hui-Xiang Liu,Yan-Li Zhang,Shu-Qi Wang
Absorbable vascular sealing medical glue, which belongs to Class III medical devices, is a special new material for preventing the leakage of cerebrospinal fluid. Medical four-arm poly(ethylene glycol)-N-hydroxysuccinimide-glutarate (4-arm-PEG-SG) with a molecular weight of 20 000 is the main component of the absorbable medical glue. According to its quality standard, the quality control of residues 1,3-dicyclohexylurea (DCU), glutaric acid (GA) and triethylamine (TEA) is required. A rapid analytical method of quantitative 1H nuclear magnetic resonance (1H NMR) for the determination of residues DCU, GA and TEA in medical 4-arm-PEG-SG was established in the present study. The peaks at δ 1.56 (4H, m), δ 2.71 (4H, t, J = 6.7 Hz), and δ 2.42 (6H, q, J = 7.2 Hz) were selected for quantifying DCU, GA and TEA, respectively, with deuterated pyridine as the solvent and tetramethylsilane as the internal standard. The 1H NMR assay was validated by several experimental parameters including specificity, linearity, accuracy, precision, robustness, limit of detection (LOD), limit of quantification (LOQ) and stability. The average recoveries obtained were in the range of 99.48–102.02% for all three residues. Compared with the HPLC and GC approaches, the proposed 1H NMR method proved to be a powerful tool for quantification due to its unique advantages of simplicity, rapidity and high robustness, especially not requiring standard compounds for calibration curve preparation.
研究领域:
医学材料学
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分析化学
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DOI
高影响因子
SENSORS AND ACTUATORS B-CHEMICAL
·
2015
·
IF 4.097
Zhu Yu,Zaiwen Tian,Zhengqian Li,Zaoli Luo,Yan Li,Yi Li,Jun Ren
In this paper, a thioacetal chemosensor 1 incorporating simultaneously a carbazole moiety and an azobenzene moiety was synthesized. Among other metal ions , Hg 2+ proved to be able to selectively induce both color and fluorescence changes of 1 . The mechanism of Hg 2+ -promoted cleavage of thioacetal was confirmed by 1 H NMR experiments. Upon the addition of Hg 2+ into the yellow CH 3 CN/H 2 O solution of 1 , the resultant azobenzene-containing thioglycolamide was precipitated from the solution as a mercuric salt, leading to a colorless solution. Therefore, a novel color change pattern was developed.
研究领域:
分析化学
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环境科学
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材料科学
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DOI
高影响因子
JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY
·
2024
·
IF 5.7
Rui Fan,Jingjing Dong,Xiaoxiao Li,Ying Chen,Zhengyu Jin,Yuxiang Bai
Reuteran is a functional homopolysaccharide comprising major (α1 → 4) and interspersed (α1 → 6) linkages whose properties and functions are directly associated with the structure. In order to enrich the structural variety and application prospects of reuteran, a GtfB-type 4,6-α-glucanotransferase from Limosilactobacillus mucosae L24-B (LmGtfB), which can synthesize reuteran with high-content linear (α1 → 6) linkages, was screened. LmGtfB exhibited 4,6-α-glucanotransferase activity against starch or dextrin and can synthesize both linear and branching (α1 → 6) linkages, which offered advantages in terms of source and cost. The as-produced reuteran had the highest content of linear (α1 → 6) linkages (19% in the methylation result) among the reuterans synthesized by other GtfB-type 4,6-α-glucanotransferases. A purification method was established and applied to the extraction of the core structure of the LmGtfB products. 1H NMR and enzymatic hydrolysis revealed that the core structure contains 46.24% (α1 → 6) linkages and alternating (α1 → 4)/(α1 → 6) linkages, which was formed by enzymatic transfer of maltose.
研究领域:
生物化学
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微生物学
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碳水化合物化学
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酶学
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DOI
PubMed
高影响因子
INTERNATIONAL JOURNAL OF BIOLOGICAL MACROMOLECULES
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2020
·
IF 5.162
Yue Shi,Xiao Wang,Ning Wang,Fei-Fei Li,Yu-Lin You,Shu-Qi Wang
Glioblastoma (GBM) is the most malignant central nervous system tumor, with poor prognosis. Temozolomide (TMZ) has been used as a first–line drug for the treatment of GBM for over a decade, but its treatment benefits are limited by acquired resistance. Polysaccharides from Cibotium barometz (CBPs) are polysaccharides purified from the root of Cibotium barometz (L.) J . Sm., possessing sensitizing activity. The purpose of this study was to investigate the anti–cancer effect of CBP from different processing methods on U87 cells using a 1 H NMR–based metabolic approach, complemented with qRT–PCR and flow cytometry, to identify potential markers and discover the targets to explore the underlying mechanism. Cibotium barometz is usually processed under sand heating in clinical applications. Polysaccharides from both the processed (PCBP) and raw (RCBP) C. barometz were prepared, and the effect on enhancing the sensitivity to TMZ was investigated in vitro. CBP can significantly increase the toxicity of TMZ to the U87 cell line, promote apoptosis, enhance cell cycle changes, and arrest cells in S phase, and RCBP demonstrated better activity. Multivariate statistical analyses, such as principal component analysis (PCA) and orthogonal projection to latent structure with discriminant analysis (OPLS–DA), were used to identify metabolic biomarkers, and 12 metabolites in the cell extract samples were clearly identified as altered after RCBP exposure. NMR–based cell metabolomics provided a holistic method for the identification of CBP's apoptosis–enhancing mechanisms and the exploration of its potential applications in preclinical and clinical studies.
研究领域:
肿瘤学
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药理学
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代谢组学
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生物医学研究
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产品关联
DOI
PubMed
高影响因子
INTERNATIONAL JOURNAL OF BIOLOGICAL MACROMOLECULES
·
2020
·
IF 5.162
Jie Hao,Fangxia Wu,Rong Tang,Yuanyuan Sun,Dehua Liu,Zhenqing Zhang
Oxidized starch (oxStarch) is a major derivative of starch. In present study, 4-acetamide-TEMPO system was firstly applied to prepare specifically oxidized starch, homogeneous 1,4-linked α-D-glucuronan. The impact of oxidant amount, 4-acetamide-TEMPO amount and reaction temperature on the properties of products were investigated. The product structures were characterized with 1 H NMR for degree of oxidation (DO), SEC-MALS for MW, MS for analysis of oxidized oligosaccharides , and in-source fragmented MS for analysis of oxidized polysaccharides . The results showed that the DO of oxStarches increased, but their MWs decreased with the raise of oxidant amount; higher 4-acetamide-TEMPO amount provided higher efficiency of specific oxidation of starch, in which the product has higher DO and MW; no significant difference have been observed between the oxStarches oxidized at 4 and 25 °C, but significant degradation was observed at 50 °C. In each product, having a MW distribution, the portion with smaller size has higher DO. While some unspecific oxidation was still observed observed on the second hydroxyl groups of sugar ring in the following order of priority, position 3 > 2 > 1 > 0.
研究领域:
化学
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材料科学
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分析化学
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产品关联
DOI
PubMed
高影响因子
TOXICOLOGY LETTERS
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2018
·
IF 3.166
Ling-Yu Ruan,Jun-Ting Fan,Wei Hong,He Zhao,Ming-Hui Li,Lei Jiang,Yong-Hong Fu,Yue-Xiao Xing,Cheng Chen,Jun-Song Wang
Isoniazid (INH) is a well-known therapeutic and preventive agent against tuberculosis. However, high rates of side effects with various symptoms concerning hepatotoxicity and neurotoxicity have been reported, hindering its wide and safe application in clinic. In this investigation, rats were intoxicated with INH by gavage at doses of 200 and 400 mg/kg for 7 consecutive days to develop a rat model of acute INH-induced toxicity, which was investigated by a 1 H NMR-based metabolomics complemented with clinical assays, histopathological inspection and western blotting. INH decreased the weights of dosed rats and induced seizure and hepatic steatosis dose-dependently. Orthogonal signal correction partial least-squares discriminant analysis (OSC-PLS-DA) of the NMR profiles of rat livers, brains and serum revealed that INH dose-dependently induced oxidative stress, disorders of excitatory and inhibitory amino acid neurotransmitters, and disturbances of energy metabolism and osmotic balance, which could help clarify the mechanisms of INH-induced hepatotoxicity and neurotoxicity. This integrated metabolomics approach showcased its ability to characterize the global metabolic status of organism, providing a powerful and feasible tool to probe drug induced toxicity or side effects.
研究领域:
药理学
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毒理学
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代谢组学
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产品关联
DOI
PubMed
高影响因子
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
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2025
·
IF 3.8
Xie Baogang,Zhan Dujuan,Wu Le,Wang Lele,Lei Yongrong,Liu Meng,Liu Xiaodan,Li Suping
Congenital heart disease (CHD) poses significant clinical challenges due to limitations in early prenatal diagnosis. This study aimed to identify serum metabolic biomarkers for CHD using a combined metabolomics approach. Serum samples from 55 pregnant women carrying fetuses with confirmed CHD (CHDP group) and 49 healthy controls (ZCP group) were analyzed via non-targeted 1 HNMR metabolomics, revealing distinct metabolic profiles. Six choline pathway metabolites were further quantified by ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Among these, N,N-dimethylglycine (DMG) exhibited the most significant reduction in the CHDP group (1.07 ± 0.03 vs. 1.55 ± 0.04 µg/mL, p < 0.001), with an area under the ROC curve (AUROC) of 0.883 in the discovery cohort. Validation in an independent cohort (58 CHDP vs. 62 ZCP) confirmed DMG’s diagnostic potential (AUROC = 0.818). While betaine-homocysteine methyltransferase 2 (BHMT2) activity showed no intergroup differences, DMG’s consistent performance highlights its utility as a non-invasive biomarker. This study underscores the clinical value of metabonomics in prenatal CHD screening and establishes DMG as a promising diagnostic marker, potentially improving early detection and perinatal management. Graphical abstract
研究领域:
代谢组学
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儿科心脏病学
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产前诊断
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生物医学研究
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF HAZARDOUS MATERIALS
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2020
·
IF 9.038
Can Cheng,Jianjun Li,Jinyan Cao,Jiaxiu Guo,Wanglai Cen
The absorption properties of N-(2-hydroxyethyl) morpholine (HEM), morpholine (MP) and N-(2-aminoethyl) morpholine (AEM) for SO 2 were studied using sulfolane (SUL) as solvent in this work. Among these solvent combinations, HEM/SUL shows the best cyclic absorption performance, and the capacity of HEM-SUL-40 (40 wt% of HEM and 60 wt% of SUL) to absorb 8580 mg/m 3 SO 2 (the remainder is N 2 ) is 192.18 mg/g at 293.15 K. The absorption capacity of the second cycle is 97.5% of the first absorption cycle, which is higher than 70% of the Cansolv amine solution in a commercial application with similar experimental conditions. However, MP/SUL is difficult to desorb at high temperature, and the absorption capacity of AEM/SUL is much lower than HEM/SUL and MP/SUL. According to the FTIR , 1 H NMR and 13 C NMR, all three cyclic amines have charge transfer effects with SO 2 . The structure of HEM/SUL can be recovered after heating, but MP cannot be recovered. Δ r G m ° in the reaction against HEM with SO 2 increases significantly with increasing temperature. The Δ r G m ° of HEM-SO 2 and MP-SO 2 at 353.15 K is −12.56 kJ/mol and −16.29 kJ/mol, respectively, which further explains the easy desorption of HEM-SO 2 and the difficult desorption of MP-SO 2 at high temperature.
研究领域:
化学工程
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环境科学
·
物理化学
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产品关联
DOI
PubMed
高影响因子
ACS Applied Polymer Materials
·
2024
·
IF 4.4
Yunfei Liu,Yayu Feng,Yue Sun,Meijing Zhang,Pengfei Zhang,Ronghui Zhao,Kuilin Deng
In this investigation, a nonconjugated fluorescent polyamide with piperazine and valerolactam moieties (PAM–PV) has been synthesized by the modified Ugi polymerization using 1,4-bis(3-aminopropyl)piperazine, levulinic acid, and 1,4-bis(3-isocyanopropyl)piperazine as monomers. In the polymerization, the special construction of levulinic acid leads to the formation of valerolactam on PAM–PV chains via the Mumm rearrangement. PAM–PV shows a strong fluorescence emission at 428 nm due to the intramolecular aggregation of piperazine and valerolactam moieties along the backbone. Impressively, PAM–PV can specifically detect NO2– ions via static quenching with a linear range of 10–6–10–5 M and a detection limit of 0.6 μM (0.0276 mg/L), which was far less than the minimum allowable concentration of 3 mg/L for NO2– in drinking water specified by WHO. Furthermore, the several common anions and cations have no interference effects on the specific detection of PAM–PV to NO2– ions. The quenching mechanism of NO2– and PAM–PV by FTIR, UV, and 1H NMR measurements indicates that the strong electrostatic interaction between NO2– and PAM–PV makes the macromolecular chains more relaxed and outstretched, leading to a formation of a nonfluorescent complex. Moreover, the practical detection of NO2– in the three water bodies, sauerkraut, and ham sausage and the fabrication of a portable detecting paper to NO2– ions were conducted in this experiment.
研究领域:
聚合物化学
·
分析化学
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环境科学
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产品关联
DOI
高影响因子
DALTON TRANSACTIONS
·
2014
·Vol. 43
·期 24
·9216-9225
·
IF 4.097
Qiong Wu,Tianfeng Chen,Zhao Zhang,Siyan Liao,Xiaohui Wu,Jian Wu,Wenjie Mei,Yanhua Chen,Weili Wu,Lingli Zeng,Wenjie Zheng
Two arene Ru(II) complexes coordinated by 2-(3-methoxyphenyl)imidazole[4,5-f][1,10]phenanthroline, [(η6-RC6H5)Ru(m-MOPIP)Cl]Cl (R = H, 1; R = CH3, 2), have been prepared under microwave irradiation; the crystal structure of 2 exhibits a typical “piano stool” conformation, with bond angles for N1–Ru1–Cl1 86.02 (14)° and N2–Ru1–Cl1 84.51 (14)°. The Ru–C distance for the Ru atom bound to the benzene ring is about 0.2178(8) nm, and the average Ru–N distance for Ru atom to the two chelating N atoms is about 0.2092(4) nm. The evaluation of in vitro anticancer activities revealed that these synthetic Ru(II) complexes selectively inhibited the growth of HepG2 hepatocellular carcinoma cells, with low cytotoxicity toward LO2 human normal liver cells. The results demonstrated that the complexes exhibited great selectivity between human cancer and normal cells by comparing with the ligand m-MOPIP. Furthermore, complexes 1 and 2 could bind to c-myc G4 DNA in groove binding mode in promising affinity, and the insertion of the methyl groups in the arene ligand contributed to strengthen the binding affinity. This was also confirmed by molecular docking calculation and 1H NMR analysis which showed that both 1 and 2 can bind in the loop constructed by A6–G9 and G21–A25 base pairs in c-myc G4 DNA to block the replication of c-myc oligomer. Taken together, these results suggest that arene Ru(II) complexes display application potential as small molecule inhibitors of c-myc G4 DNA.
研究领域:
无机化学
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药物化学
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癌症研究
·
DNA相互作用
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产品关联
DOI
PubMed
高影响因子
Arabian Journal of Chemistry
·
2017
·
IF 4.553
Gang Chen,Jiaheng Lei,Yong Du,Xiaodi Du,Xuebing Chen
A novel polycarboxylate superplasticizer (PCE) with a long polyoxyethylene (PEO) chain and a terminal carboxylic group was synthesized from a modified polyether (SAE-IPEG) to increase its performance in cement. The molecular structure of the PCE was characterized by infrared spectroscopy and 1 H nuclear magnetic resonance (NMR) spectroscopy. The performance of synthesized PCE in cement was studied in the absence and the presence of montmorillonite (Mmt) clay. It was found that the PCE disperses in cement uniformly without aggregation, which is different significantly from the conventional PCEs. Adsorption measurements and X-ray diffraction analysis revealed that the synthesized PCE only interacted with Mmt via surface adsorption, whereas the conventional PCEs interact with the clay through the surface adsorption and the chemical intercalation. Such dramatic change could be ascribed to the introduction of an electronegative carboxylic acid group as a terminal group into the long polyoxyethylene chain of PCE, which reduced the adsorption and enhanced tolerance of PCE on Mmt.
研究领域:
材料科学
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化学工程
·
土木工程
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产品关联
DOI
高影响因子
危险品化学品经营许可证（带存储）