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MICROCHEMICAL JOURNAL · 2023 · IF 4.8

Hexafluoroisopropanol-based supramolecular solvent for liquid phase microextraction of triazole fungicides in drinking water and beverages

Ruiyu Fu,Tingze Ren,Yanhui Zhang,Qingxin Lu,Xiaoli Guo,Xin Di

A new supramolecular solvent (SUPRAS) was synthesized using hexafluoroisopropanol (HFIP) as hydrogen bond donor and undecanol as hydrogen bond acceptor. Then SUPRAS was used as extraction solvent to enrich triazole fungicides in drinking water and beverages by liquid phase microextraction (LPME). Additionally, several variables that influence extraction efficiency were optimized, and the significant factors were investigated by Box-Behnken design. At optimum condition, the method shows desirable precision (RSDs less than 19.4%) and acceptable recovery (63.4%-112.1%). The low limits of detection and limits of quantitation of this method were found to be in the range of 1.0–5.0 μg/L and 5.0–20 μg/L, respectively. Compared with other analytical techniques, the method demonstrated comparable sensitivity, consumed less extractant (750 μL) and a shorter pre-treatment time (10 min). The formation mechanism of SUPRAS was investigated by density functional theory. The proposed methodology was green, sensitive, time-saving and successfully applied to determine triazole fungicides in drinking water and beverages, making it an alternative technique for the analysis of trace analytes with satisfactory sensitivity.

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Polymers · 2021 ·Vol. 13 ·期 22 ·3906 · IF 4.329

Fiber Nanoarchitectonics for Pre-Treatments in Facile Detection of Short-Chain Fatty Acids in Waste Water and Faecal Samples

Guozhe Deng,Li Xie,Shengjia Xu,Xuejun Kang,Jizheng Ma

Short-chain fatty acids (SCFAs) are among the active metabolites in biological process both in the intestinal tract and the bioconversion of organic wastes, which has resulted in various human diseases and environmental problems. In order to accurately detect SCFAs, we introduced a novel extraction sorbent. Electrospun polyacrylonitrile (PAN) nanofiber membrane was synthesized, then poly (3, 4-Ethylenedioxythiophene) (PEDOT) was deposited onto the surface of electrospun PAN nanofibers by in situ polymerization. The morphology of the composite PAN/PEDOT nanofiber was characterized by scanning electronic microscopy (SEM) and FTIR spectrum. PAN/PEDOT was used to isolate and concentrate the SCFAs in waste water and fecal samples before gas chromatography mass spectrometry (GC-MS) analysis. The analytical method was evaluated systematically, and low limits of detection (LODs) of 0.34–0.87 μg/L and good linearity (R2≥ 0.9953) were obtained. The method was applied successfully for the determination of SCFAs in waste water and fecal samples, with good recovery (87.5–104.6%) and satisfactory reproducibility (relative standard deviation: 6.5–14.1%). The results indicated that the proposed method can be used as a potential approach for the determination of SCFAs with high sensitivity in waste water and biological samples.Keywords:adsorbent;conducting polymer;electrospinning;polyacrylonitrile;solid phase extraction

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JOURNAL OF CHROMATOGRAPHY A · 2021 · IF 4.759

Simultaneous quantification of eleven short-chain fatty acids by derivatization and solid phase microextraction - Gas chromatography tandem mass spectrometry

Zhibo Fu,Qiangqiang Jia,Hongyang Zhang,Lu Kang,Xuezhi Sun,Min Zhang,Yuerong Wang,Ping Hu

As metabolites of the gut microbiome, short-chain fatty acids (SCFAs) played an important role in the diagnosis of the metabolic diseases. Because of the high polarity, high volatility and complex matrix of biological samples, the highly sensitive, selective and accurate method to determine SCFAs remains a major challenge. Herein, a new method for simultaneous quantification of eleven SCFAs by derivatization combined with solid phase microextraction (SPME) and gas chromatography tandem mass spectrometry (GC–MS/MS) was developed. Isobutyl chloroformate coupled with isobutanol was used as the reaction reagent to derivatize SCFAs. The method validation data showed a satisfactory linearity with the linear regression coefficients (R) ranging from 0.9964 to 0.9996. The limit of detection (LOD) of all SCFAs ranges from 0.01 ng·mL −1 to 0.72 ng·mL −1 and the limit of quantification (LOQ) ranges from 0.04 ng·mL −1 to 2.41 ng·mL −1 . The intra-day and inter-day precision (RSDs) ranged from 0.65% to 8.92% and 1.62% to 15.61%, respectively. The recovery ranged from 88.10% to 108.71%. Finally, the developed method was successfully used to determine SCFAs in mice fecal sample, and ten of the SCFAs were found in feces of mice, including formic acid.

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MICROCHEMICAL JOURNAL · 2023 · IF 4.8

Development of self-dispersion ferrofluid-based dispersive liquid–liquid microextraction for determining chiral fungicide hexaconazole in water, tea, and juice using high-performance liquid chromatography

Xiaojiao Zheng,Weiwei Ma,Qihui Wang,Yaping Xu,Yukun Yang,Shu Qin,Xu Jing

In this study, a fast, green, and efficient ferrofluid-based dispersive liquid–liquid microextraction (DLLME) method was developed for determining chiral fungicide hexaconazole residues using high-performance liquid chromatography (HPLC). The ferrofluid as extraction solvent was composed of deep eutectic solvents (DESs) and Fe 3 O 4 , in which DES as the functional support solvent of the ferrofluid was synthesized by fenchol, hexanoic acid, and acetic acid in the molar ratio of 1:0.5:3. The prepared ferrofluid is characterized by self-dispersion and magnetism, which can eliminate the vortex, ultrasound, and centrifugation steps. Chiral separation and detection of hexaconazole enantiomers were performed by HPLC. Under optimal conditions, linearity ranged between 0.02 and 2 μg mL −1 , the limit of detection (LOD) was 0.006 μg mL −1 , and relative standard deviations were less than 8.6 %. The recoveries in the water, tea, and juice ranged from 83.0 % to 101.7 %. The proposed self-dispersion ferrofluids can facilitate the development of fast microextraction methods for pesticides in food samples.

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ACS Catalysis · 2023 · IF 12.9

Nanostructured PtBi Alloy Enables Direct Oxidation of Linear α-Alcohols to Fatty Acids

Luyao Guo,Xiaoyan Liu,Ziang Zhao,Ronghe Lin,Yu Meng,Xinzheng Ma,Yihui Li,Xiaoling Mou,Li Yan,Hejun Zhu,Yunjie Ding

Nanostructured bimetallic Pt–Bi catalysts are designed by defect engineering of N-doped carbons as the hosts. The optimal catalyst delivers good yields (>98%) in the direct oxidation of C5–C9 linear α-alcohols to corresponding fatty acids, significantly outperforming activated carbon-supported benchmarks and rivaling the state-of-the-art systems. A combined kinetic and computational study on n-heptanol oxidation as a model reaction unveils the kinetic and thermodynamic origins of the better performance of the PtBi alloy than neat or Bi-modified Pt(111) surfaces. Structure–performance correlations further identify that the metal particle size, surface Bi/Pt ratio, and strong basicity strongly influence the catalyst performance in alcohol oxidation. The creation of nitrogen defects facilitates the formation of the surface PtBi alloy and brings strong basicity, accounting for the boosted performance. These findings enable a step closer toward the manufacture of valuable fatty acids from abundant coal by coupling the advanced oxidation with the recently piloted higher alcohol synthesis via the Co–Co2C-catalyzed Fischer–Tropsch reaction.

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FOOD CHEMISTRY · 2023 · IF 8.8

Determination of chiral prothioconazole and its chiral metabolite in water, juice, tea, and vinegar using emulsive liquid–liquid microextraction combined with ultra-high performance liquid chromatography

Xingle Guo,Xiaojiao Zheng,Xu Guo,Junxue Wu,Xu Jing

Emulsive liquid–liquid microextraction (ELLME), a simple, rapid, and environmentally friendly technique, was established to identify chiral prothioconazole and its chiral metabolite in water, juice, tea, and vinegar using ultra-high-performance liquid chromatography (UPLC). Environmentally friendly extractant was mixed with pure water to prepare a high-concentration emulsion, which was added to samples to complete the emulsification and extraction in 1 s. Afterward, an electrolyte solution was added to complete the demulsification without centrifugation. ELLME did not use dispersants compared to the familiar dispersive liquid–liquid microextraction (DLLME), thus reducing the use of toxic solvents and avoiding the effect of dispersants on the partition coefficient. The linear range was from 0.01 to 1 mg/L. The limit of detection was 0.003 mg/L. The extraction recoveries ranged from 82.4 % to 101.6 %, with relative standard deviations of 0.7–5.2 %. The ELLME method developed has the potential to serve as an alternative to DLLME.

✓ 已验证 产品关联 DOI PubMed 高影响因子
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LANGMUIR · 2023 · IF 3.9

Phase Transitions of Naphthalene-2,3-carbonitride Steered by Solvent Effects and Metal Ion Concentration Variation

Longnan Yu,Sihao Li,Yan Lu,Zhongping Wang,Mingming Fu,Sheng Wei,Changgang Xu,Qing Wang,Xiaoqing Liu,Li Wang

The delicate regulation of structural phase transition can provide advanced approaches for fabricating desired and well-organized nanoarchitectures on surfaces. Introduction of metal ions into pure organic systems can facilitate the phase transition from hydrogen-bonded structures to metal–organic structures by coordinating with organic molecules. However, it remains a challenge to attain a phase transition dominated by variable metal coordination configurations through adjustment of the metal ion concentration. Herein, we report the phase transitions of naphthalene-2,3-carbonitride (2,3-DCN) molecules on highly oriented pyrolytic graphite (HOPG) under varying solvents and Cu2+ ion concentrations. By integrating data from scanning tunneling microscopy imaging and density functional theory calculations, it is demonstrated that phase transitions of 2,3-DCN occur through forming diverse coordination configurations where Cu2+ ions can coordinate with 2,3-DCN and 1-nonanoic acid or Cl– ions to form different ligand components with a coordination number of 4 when varying the molar ratios of 2,3-DCN to Cu2+ ion in the 1-nonanoic acid solvent. However, in the case of 1-heptanoic acid as a solvent, the self-assembly structure of 2,3-DCN only changes via the alteration of hydrogen bonding sites and Cu2+ ions do not coordinate with 2,3-DCN molecules. These findings provide valuable insights into the coordination behavior of metal ions in different solvents.

CAS / MDL: 111-14-8 112-05-0
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JOURNAL OF PHARMACEUTICAL SCIENCES · 2021 · IF 3.534

Anti-CD19 mAb modified mesoporous titanium dioxide as exclusively targeting vector for efficient B-lymphoblastic leukemia therapy

Shanshan Li,Long Zhang,Mingda Li,Jiao Huang,Baocheng Cui,Jie Jia,Zhaoming Guo,Kun Ma,Changhao Cui

B lymphoblastic leukemia (B-LL) is a clonal hematopoietic stem cell neoplasm derived from B-cell progenitors, which mainly occurs in children and adolescents and is one of the main causes of death from malignant tumors in this population. The surface marker CD19 is specifically expressed on the membrane of most malignant B-cells, which is widely used as a marker of B-LL antigen-specific immunotherapy . In this study, mesoporous titanium dioxide nanoparticles (MTNs)-based antibody drug delivery system was designed for B-LL treatment. Anti-CD19 monoclonal antibody was conjugated to PEGylated MTNs, and doxorubicin (DOX) was loaded in the nanoparticle . The CD19-PEG-MTN/DOX nanoparticle could recognize CD19 + B -LL cell lines and induced them apoptosis, but nontoxic for the normal cells. Further, after treated with CD19-PEG-MTN/DOX nanoparticle, pro-apoptotic proteins Bax and Caspase-3 in KOPN 8 and NALM-6 cells were significantly upregulated, but anti-apoptotic proteins Bcl2 , MCL-1, HSP 70, and BAG 3 were downregulated, which indicated the activation of the apoptosis pathway by the nanodrug. By contrast, CD19-PEG-MTN/DOX didn't play a part on CD19 − cell line U937. Besides, the cytotoxicity of CD19-PEG-MTN/DOX was low with good biocompatibility. Collectively, CD19-PEG-MTN/DOX is a promising antitumor nanodrug for the treatment of B-LL.

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TALANTA · 2021 · IF 6.057

A novel charge derivatization-direct infusion mass spectrometry method for the quantitative analysis of C1–C8 fatty acids in rubber seed oil-based biodiesel

Hua-Ming Xiao,Yan Shi,Yong-Xue Yang,Shuai Zhao,Xian Wang

The free fatty acids that contain one to eight carbons (C 1 –C 8 ) in biodiesel would affect the quality of biodiesel. It is still a matter of challenge to simultaneously determine the composition of C 1 –C 8 fatty acids in seed oil and seed oil-based biodiesel. Herein, a novel method of charge derivatization coupling with direct infusion mass spectrometry (CD-DIMS) was developed for the determination of the C 1 –C 8 fatty acids in biodiesels. A fixed-charge derivatization reagent, 1-cyclohexyl-3-(2-morpholinoethyl)carbodiimide (CMCT), was used to convert fatty acids into their cationic derivatives, which significantly improved the sensitivity and selectivity of detection. Good linearity was observed with the limits of detection (LODs) in the range of 0.0002–0.001 μg mL −1 for the investigated fatty acids. The recovery was in the range of 85.1%–101.9% and the matrix effect was within the range of 75.5–93.2%. The developed method was carried out to analyze C 1 –C 8 fatty acids in rubber seed oil (RSO) and RSO-based biodiesels produced by different catalysts, including NaOH, TiO 2 , and carbodiimide . It was also applied to the dynamic monitoring of C 1 –C 8 fatty acids in RSO and produced RSO biodiesels during the oxidation process. As results, formic acid , acetic acid, and propionic acid were detected in aged RSO and biodiesel samples. The contents of formic acid, acetic acid, and propionic acid all increased in aged RSO and biodiesels, but with different growth rates. These results demonstrated that the developed CD-DIMS method can provide a quick, accurate, and sensitive analysis of C 1 –C 8 fatty acids in seed oil and biodiesel samples.

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JOURNAL OF ASIA-PACIFIC ENTOMOLOGY · 2020 · IF 1.101

Development of lady beetle attractants from floral volatiles and other semiochemicals for the biological control of aphids

Jinhao Zhao,Zhongyan Wang,Zhongshan Li,Jiayu Shi,Ling Meng,Guorong Wang,Jingli Cheng,Yongjun Du

Aphids are among the most destructive phytophagous pests of host plants, because of their rapid reproduction, parthenogenesis, extensive crop damage, and the transmission of many plant viruses. Since lady beetles are important predatory natural enemies of aphids, developing lady beetle attractants to increase their field abundance is vital for aphid control. Floral volatiles and other semiochemicals are reportedly attractive to lady beetles. In this research, a total of 58 floral volatiles were tested by Y-tube olfactometer assays, among which 29 were highly attractive to both Harmonia axyridis (Coleoptera: Coccinellidae) and Coccinella septempunctata (Coleoptera: Coccinellidae). Meanwhile, the results of wind tunnel trials showed that only isoamyl acetate, α -humulene, trans -3-hexen-1-ol, methyl salicylate, and β -pinene lure these two species. Thereafter, 15 semiochemicals from pests, natural enemies, and pest-infested crops were mixed with the selected floral volatiles, to determine optimum formulations for attracting lady beetles through wind tunnels and further field trials. Eventually, formulas (1) α -humulene: β -pinene: methyl salicylate: trans -3-hexen-1-ol = 1:3:3:10; (5) α -humulene: β -pinene: methyl salicylate:1-nonanal = 1:3:3:10; (8) α -humulene: β -pinene: methyl salicylate: indole = 1:3:3:10 ( 1 , 5 , and 8 are labels used for the various formulations in field trials) were successfully verified to be attractive to lady beetles in both pumpkin and wheat fields. These formulations will be of great significance in developing integrated pest management strategies for aphid control.

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FUEL · 2020 · IF 5.578

Green synthesis of ester base oil with high viscosity – Part Ⅰ: Catalyst preparation, characterization, evaluation, and mechanism analysis

Shaojian Hu,Jianhua Zhu,Bencheng Wu,Rui Ma,Yuechun Chang,Xiaohui Li,Yuqing Wei,Liujie Yu

High viscosity ester base oil, as an eco-friendly lubricant base oil with high performance, can significantly reduce the friction, wear, and energy consumption of large machinery. However, there is less research on the preparation of heterogeneous catalysts for synthesis of high viscosity ester oil. In this work, Sn/Zr mixed oxide catalysts were prepared for the green synthesis of ester base oil with high viscosity. This approach gets rid of additional template, surfactant, organic solvent, sulfur, nitrogen, phosphorus, and halogen, thereby avoiding the potential environmental pollution. A superior powdered catalyst MO-Sn 8 Zr-9.0-160-18 was developed with optimized Sn/Zr molar ratio, pH, hydrothermal temperature, and hydrothermal time of 8:1, 9.0, 160 °C, and 18 h, respectively. Results of catalyst characterization indicated that the developed catalysts were mesoporous materials with hydrophobic properties, allowing for free diffusion of macromolecules, adsorption of reactants, and desorption of water. Additionally, the specific surface area, pore volume, pore diameter, and surface hydrophobicity of catalyst were enhanced by doping Zr, so the catalysts with higher [Sn/Zr] ICP /[Sn/Zr] XPS exhibited better catalytic activity. Preformed catalyst was prepared by simple mechanical mixing method to achieve better catalyst separation. The specific surface area, acid amount, and acid strength of catalyst were indeed improved significantly after catalyst molding. By programmed heating, the preformed catalyst achieved a maximum carboxyl conversion of 97.2%. Moreover, spent catalyst could be reactivated via solvent washing, drying, calcination, and hydrogen reduction, exhibiting good reusability.

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NEW JOURNAL OF CHEMISTRY · 2020 ·Vol. 44 ·期 25 ·10621-10627 · IF 3.288

A novel column fabrication approach for capillary gas chromatography via a cross-linked organogel network with high stability and inertness

Xue Xiong,Meiling Qi

This work presents a novel column fabrication approach for capillary gas chromatography (CGC) through the condensation reaction of a hydroxyl-terminated polymer with a cross-linker inside a capillary column. In this work, polypropylene glycol (PPG 4000) and tris[3-(trimethoxysilyl)propyl]isocyanurate (ICS) were employed to fabricate the PPG-gel capillary column for GC analyses. Inside the column, a 3D cross-linked organogel network forms on the capillary inner surface by condensation of PPG 4000 with ICS under the given mild conditions. As a result, the PPG-gel column exhibited moderate polarity and showed distinctly advantageous resolving performance and inertness for carboxylic acids over the PPG column by the conventional static coating method. Also, it achieved high-resolution separations of the isomer mixtures of alkanes, alkylbenzenes and halobenzenes. Moreover, the PPG-gel column exhibited dramatically improved solvent stability because of its cross-linked organogel network. The organogel column displayed excellent column repeatability and reproducibility with the RSD% values in the range of 0.01–0.04% for run-to-run, 0.71–0.84% for day-to-day and 2.4–3.1% for column-to-column. The proposed organogel approach is facile and applicable to other analogous materials and has a promising future for wide applications.

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