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CHROMATOGRAPHIA · 2012 ·Vol. 75 ·期 5 ·289-296 · IF 1.195

A Silica Monolithic Column with Chemically Bonded l-Pipecolic Acid as Chiral Stationary Phase for Enantiomeric Separation of Dansyl Amino Acids by CEC–MS

Zhang Yulin,Huang Liang,Chen Qinhua,Chen Zilin

A silica monolithic column chemically modified with l -pipecolic acid as chiral stationary phase has been developed for chiral separation of dansyl amino acids by capillary electrochromatography–mass spectrometry (CEC–MS). The monolithic column was prepared by a sol–gel process and subsequent chemical modification by l -pipecolic acid as chiral selector with 3-glycidoxypropyltrimethoxysilane as spacer. Interestingly, it was found that the l -pipecolic acid-modified monolithic column can hold copper(II) ions tightly after loading Cu(II) ions during column preparation and conditioning and allows CEC separation to be conducted based on chiral ligand exchange with MS detection by a mobile phase without copper ions. It has been demonstrated that the chiral monolithic column operates well for enantioseparation of several dansyl amino acids by CEC–MS.

研究领域: 分析化学 · 药物化学
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ACS Applied Polymer Materials · 2023 · IF 5

Retarded Interfacial Formation of Polyamine-Based Nanofiltration Membranes with Pyromellitic Acid: Separation, Acid Stability, and Antifouling Performance

Kayode Hassan Lasisi,Kaisong Zhang

Crosslinked and additive-added polyamide thin-film composite (TFC) nanofiltration (NF) membranes formed by the conventional interfacial polymerization (IP) process have shown good performances. However, studies on polyamine TFC NF membrane prepared via an adjusted IP process with low-cost acid ligands as an interfacial additive for improved liquid-based separation are still lagging. In this regard, a polyamine-based TFC NF membrane synthesized by retarding the interfacial polymerization (IP) process with pyromellitic acid (PMA) (a polycarboxylate acid ligand) is herein reported. The PMA-adjusted membrane displayed a superb range of pure water fluxes from 9.8 to 20.4 L m–2 h–1 bar–1, with the best-performed membrane achieving up to 95.1% for Na2SO4 rejection. Thus, the water permeability of the PMA-TFC membrane is ∼2.4 times as high as the control TFC membrane. The best-performed PMA-TFC membrane showed good hydrophilicity, pressure resistance, and long-term filtration stability. In addition, the membrane structural stability was maintained with ∼3.9% declination in salt rejection after 30 days of immersion in 0.1 M HNO3 solution. Also, an impressive fouling resistance was achieved after three-cycle of bovine serum albumin fouling tests. This work, therefore, offers a more feasible way of designing polyamine-based NF membranes with good prospects in water reuse and nitric acid-generating wastewater treatment application.

研究领域: 材料科学 · 环境工程
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Evidence-based Complementary and Alternative Medicine · 2022 · IF 2.65

Potential Plasma Metabolic Biomarkers of Tourette Syndrome Discovery Based on Integrated Non-Targeted and Targeted Metabolomics Screening

Leying Xi,Fuqiong Zhou,Wenxiu Ji,Weina Zhu,Jie Ruan,Yajie Zhang,Xueling Hu,Hongyan Long

Objective. Tourette syndrome (TS) is a chronic neuropsychiatric disorder characterized by abnormal movements, phonations, and tics, but an accurate TS diagnosis remains challenging and indeed depends on its description of clinical symptoms. Our study was conducted to discover and verify some metabolite biomarkers based on nontargeted and targeted metabolomics. Methods. We conducted untargeted ultrahigh-performance liquid chromatography-quadrupole time-of-flight mass spectrometry (UHPLC-Q-TOF/MS) for preliminary screening of potential biomarkers on 30 TS patients and 10 healthy controls and then performed validation experiments based on targeted ultrahigh-performance liquid chromatography triple quadrupole-MS (UHPLC/MS/MS) on 35 TS patients and 14 healthy controls. Results. 1775 differentially expressed metabolites were identified by partial least squares discriminant analysis (PLS-DA), fold-change analysis, T-test, and hierarchical clustering analysis (adjusted value <0.05 and |logFC| > 1). TS plasma samples were found to be differentiated from healthy samples in our approach. Furthermore, aspartate and asparagine metabolism pathways were considered to be a significant enrichment pathway in TS progression based on metabolite pathway enrichment analysis. For the 8 metabolites involved in this pathway that we detected, we then performed validation experiments based on targeted UHPLC/MS/MS. The t-test, Mann–Whitney U test, and receiver operating characteristic (ROC) curve analysis were used to determine potential biomarkers. Ultimately, L-arginine and L-pipecolic acid were validated as significantly differentiated metabolites (), with an AUC of 70.0% and 80.3%, respectively. Conclusion. L-pipecolic acid was defined as a potential biomarker for TS diagnosis by the combined application of nontargeted and targeted metabolomic analysis.

研究领域: 医学 · 神经科学 · 代谢组学
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CHEMICAL PAPERS · 2022 ·Vol. 77 ·期 1 ·259-268 · IF 2.146

Functional ionic liquids as chiral selector for visual chiral sensing and enantioselective precipitate

Ma Xiaofei,Zhang Chengchen,Cai Liangliang

This work describes a rapid and efficient method for visual chiral recognition by making use of chiral ionic liquids (CILs) based on shikimic acid and D-pipecolinic acid. Cooperation between copper (II) and appropriate solvents resulted in visual enantioselectivity responses of several amino acids and mandelic acid. All the enantiomeric distinguishment could be obtained within 3 min, depending on the difference of colour or solubility. Then, scanning electron microscopy, infrared spectroscopy, ultraviolet spectroscopy, thermogravimetric analysis and elemental analysis were employed to investigate the potential recognition mechanism. The results indicated that chiral recognition was strongly associated with the different stability between D-complex and L-complex. Furthermore, separation was achieved by treating the chiral sensor with racemic compounds. In the case of tryptophan, the proposed method provided good enantiomeric excess values (90.7% in solid phase and 63.2% in liquid phase). Graphical abstract

研究领域: 分析化学 · 材料科学 · 手性
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Parasites & Vectors · 2022 ·Vol. 15 ·期 1 ·1-12 · IF 4.047

Multiple biochemical indices and metabolomics of Clonorchis sinensis provide a novel interpretation of biomarkers

Qiu Yang-Yuan,Chang Qiao-Cheng,Gao Jun-Feng,Bao Ming-Jia,Luo Hai-Tao,Song Jin-Ho,Hong Sung-Jong,Mao Rui-Feng,Sun Yun-Yi,Chen Ying-Yu,Liu Ming-Yuan,Wang Chun-Ren,Liu Xiao-Lei

Background Clonorchiasis, an infectious disease caused by the liver fluke Clonorchis sinensis , may lead to the development of liver and gallbladder diseases, and even cholangiocarcinoma (CCA). However, the pathogenesis, host-pathogen interaction, and diagnostic markers for clonorchiasis remain unclear. Methods Eighteen rabbits were randomly divided into control group ( n  = 9) and C. sinensis -infected group ( n  = 9), and their plasma samples were collected at 7, 14, 28, and 63 days post-infection (dpi). Biochemical indices and metabolites in different infection periods were detected. A non-targeted ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) approach was employed to investigate the metabolic profiles of plasma in rabbits, and related metabolic pathways of differential metabolites and correlation between candidate biochemical indices and differential metabolites were analyzed. Finally, the candidate biomarkers were verified with human samples using a targeted metabolomics method. Results The result of biochemical indices indicated C. sinensis infection would affect the liver function biochemical indices, especially alanine aminotransferase, aspartate transaminase (AST), glutamyl transpeptidase (GGT), total bile acid, high-density lipoprotein, and cholinesterase. The metabonomic results showed that 58, 212, 23, and 21 differential metabolites were identified in different phases of the infection. Multivariate statistical analysis of differential metabolites revealed distinct metabolic signatures during different phases of infection, with most of these signatures being observed at 14 dpi, which mainly influences the amino acid metabolisms. For metabolites and biochemical indices, AST, GGT, hypoxanthine, l -pipecolic acid, and d -glucuronate represented potential noninvasive biomarkers for the diagnosis of C. sinensis ( P  < 0.05 and AUC > 0.8). Furthermore, GGT and d -glucuronate levels were positively correlated with the infection ( r (28) = 0.98, P  < 0.0001) and showed excellent diagnostic performance (AUC = 0.972; 95% confidence interval, 0.921 to 1.000). Conclusions The present results provide new insights into plasma metabolic changes in rabbits during C. sinensis infection, and the potential biomarker may be used for developing an effective method to diagnose clonorchiasis in the future. Graphical Abstract

研究领域: 寄生虫学 · 代谢组学 · 医学诊断 · 传染病
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