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FOOD CHEMISTRY · 2022 · IF 9.231

Fast extraction of aflatoxins, ochratoxins and enniatins from maize with magnetic covalent organic framework prior to HPLC-MS/MS detection

Dan Wei,Ao Pan,Can Zhang,Ming Guo,Chaoyan Lou,Ju Zhang,Huizhen Wu,Xu Wang

A simple, rapid and sensitive vortex-assisted magnetic solid phase extraction (MSPE) method using core–shell structured magnetic covalent organic frameworks (Fe 3 O 4 /COF-TpBD) as adsorbents was established for simultaneous determination of aflatoxins, ochratoxins and enniatins in maize before high-performance chromatography tandem spectrometry detection. Fe 3 O 4 /COF-TpBD was facilely fabricated, characterized, and applied for simultaneous extraction of ten mycotoxins from maize. Key parameters affecting MSPE efficiency were investigated. The method possessed good linearity (0.05–50 μg/kg), high sensitivity (0.02–1.67 µg/kg for limits of detection), and satisfactory recoveries (73.8–105.3 %), with relative standard deviations less than 8.5 %. The amount of adsorbent used (5 mg) and the time required (0.5 min each for adsorption and for desorption) for MSPE were greatly shortened in comparison with the previous reports. Therefore, the fabricated Fe 3 O 4 /COF-TpBD exhibited a great potential for rapid extraction of common mycotoxins in maize, which can be attributed to its multiple interactions with the target mycotoxins.

研究领域: 分析化学 · 食品安全 · 真菌毒素分析
✓ 已验证 产品关联 DOI PubMed 高影响因子
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ANALYTICA CHIMICA ACTA · 2024 · IF 5.7

Mesoporous carbon hollow spheres based sensitive SPME probes for in vivo sampling analysis of selected plant hormones in Chinese aloes

Yan Liu,Jiajia Han,Guosheng Chen,Siming Huang,Shuyao Huang,Juan Zheng,Jianqiao Xu,Fang Zhu,Gangfeng Ouyang

Phytohormones are a class of endogenous substances that separately or synergistically regulate the growth, development, and differentiation of plants. Accurately and efficiently detecting and monitoring the concentration of plant hormones in living plants is of significant importance. Herein, a novel mesoporous carbon hollow spheres (MCHS)-based in vivo solid phase microextraction (SPME) probe was designed for in vivo sampling of plant hormones. The designed MCHS features the advantages of high surface area, porous shells, and large hollow spaces, facilitating the dynamic adsorption and enrichment of target phytohormone. In addition, a cationic polyelectrolyte, (poly (diallyl dimethyl ammonium chloride) (PDDA), was further modified onto the MCHS to expedite the extraction process by electrostatic interaction. Utilizing the MCHS@PDDA probe in combination with HPLC-MS/MS facilitated the continuous monitoring of three plant hormones (abscisic acid (ABA), indole-3-acetic acid (IAA), and gibberellin (GA3)) in Chinese aloe. The detection limit of this method was 0.016–0.090 μg/L, the linear range was 10–1000 μg/L, and both the RSD of the single probe (n = 6) and probe-to-probe test (n = 6) were less than 7.2 %. This method had excellent accuracy and good reproducibility comparable to the traditional sample pretreatment method. Ultimately, this established in-vivo SPME method was successfully adopted to quantify three selected plant hormones in living Chinese Aloes, providing a new method for the long-term monitoring of endogenous active substances in living system.

研究领域: 分析化学 · 植物科学 · 生物技术
✓ 已验证 产品关联 DOI PubMed 高影响因子
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CHEMICAL ENGINEERING JOURNAL · 2018 · IF 6.735

Degradation of methylparaben using BiOI-hydrogel composites activated peroxymonosulfate under visible light irradiation

Youyou Hu,Zhengkui Li,Jianhua Yang,Hongjie Zhu

A novel hydrogel photocatalyst (p(HEA-APTM)-BiOI) was synthesized by irradiation polymerization and chemical precipitation method, while employed as peroxymonosulfate (PMS) activator to enhance methylparaben (MP) degradation. The structure, morphology and physicochemical properties of the prepared p(HEA-APTM)-BiOI were characterized by XRD, XPS, SEM, TEM, FTIR and BET. The experimental results revealed that the MP catalytic degradation by p(HEA-APTM)-BiOI activated PMS can achieve the best performance under the visible light irradiation. In addition, the parameters including the molar radio of [PMS]/[MP], initial pH, Cl − and HCO 3 − were also investigated in detail. It was worth noting that p(HEA-APTM)-BiOI also effectively eliminated MP in the absence of visible light. Based on the quenching experiment, 1 O 2 , h + and O 2 − were determined as the dominant active species contributing to the catalytic oxidation process in the p(HEA-APTM)-BiOI/PMS/Vis system, and the possible degradation mechanism was also elaborated. Eventually, the possible pathways of MP degradation were deduced from several intermediates identified by HPLC-MS.

CAS / MDL: 10035-06-0 818-61-1
研究领域: 环境科学 · 材料科学 · 化学工程 · 光化学
✓ 已验证 产品关联 DOI 高影响因子
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TALANTA · 2022 · IF 6.556

Development of a highly sensitive and specific monoclonal antibody-based ELISA coupled with immuno-affinity extraction for the detection of anticancer drug 5-fluorouracil in blood samples

Ting Zhou,Guangzhao He,Changjia Hu,Kang Wu,Ying Liu,Jianguo Li,Anping Deng

5-Fluorouracil (5-FU) is an effective anticancer drug widely used in cancer treatment. In this study, two 5-FU derivatives containing a spacer arm with the carboxylic group at the end were synthesized, which were linked to the carrier proteins to form 5-FU-protein conjugates used as the immunogens for the production of monoclonal antibody (mAb). Based on the produced mAb, the highly sensitive and specific enzyme-linked immunosorbent assay (ELISA) for 5-FU detection was established. The IC 50 and LOD values of the assay were found to be 19.5 ng mL −1 and 0.5 ng mL −1 , respectively. There was no cross-reactivity (CR) of the ELISA with cytosine , thymine and uracil , which avoided the interference from inherent pyrimidines. The CR values of the assay with three substitutes of 5-FU (tegafur, 5-fluoro-2′-deoxyuridine, carmofur) were within 9.7%–17.6%. The produced mAb was also applied in sample extraction. The immuno-affinity column capable specific capturing 5-FU was prepared by immobilizing the mAb on Sepharose-4B gel and filling into a SPE column. The recoveries of 5-FU in spiked samples measured by ELISA were 72.4%–90.7% with RSD of 3.6%–8.3%. Five blood samples collected from patients were extracted by immuno-affinity column, then measured by ELISA and confirmed by HPLC-MS/MS. There was a good correlation between HPLC-MS/MS and ELISA. It is demonstrated that the developed ELISA combined with immuno-affinity extraction can be a powerful alternative method for the detection of 5-FU in blood samples.

研究领域: 药理学 · 分析化学 · 免疫学 · 临床化学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES · 2024 · IF 2.8

Determination of six volatile fatty acids in human serum, urine and faeces by low temperature derivatisation combined with HPLC–MS/MS

Qian Li,Yongfu Zeng,Lianfeng Ai,Maolin Wei,Xiaomeng Liu,Xiaochan Zhao,Haoran Zhang,Xiujuan Guo

A stable isotope dilution-liquid chromatography tandem mass spectrometry method based on a low-temperature derivatization strategy with 3-nitrophenylhydrazine (3-NPH) was developed for the determination of six volatile fatty acids (VFAs) in serum, urine, and feces. Ice acetonitrile was used to precipitate proteins and extract the target analytes. The extract was derivatized with 3-NPH methanol solution at 4 °C. BEH C8 (1.7 μm, 2.1 × 100 mm) column was used for chromatographic separation, and acetonitrile–water (both containing 0.01 % formic acid) were used as the mobile phase with a gradient elution of 10 min. Electrospray ionization source (ESI) in negative ion multiple reaction monitoring (MRM) mode were used for analyte detection. The regression coefficients R 2 of the calibration curves for the six VFAs were in the range of 0.9963–0.9994, and the LOQs were in the range of 0.02–0.5 μg mL −1 , with the recoveries in the range of 85.3–104.3 %, and the intra- and inter-day precision in the range of 1.8–9.1 %. The method is simple, accurate and reliable, and has been applied in the sensitive determination of VFAs in complex biological samples.

研究领域: 分析化学 · 生物医学
✓ 已验证 DOI PubMed 高影响因子
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JOURNAL OF CHROMATOGRAPHY A · 2024 · IF 3.8

Preparation of magnetic amphiphilic resin microspheres via the one-step polymerization method and extraction of four glucocorticoids for HPLC–MS analysis

Zibo Zhou,Liang He,Tianyi Wang,Hongzhen Tang,Suzi Qin,Xueyan Nan,Wenbo Cheng,Haibo He,Pengli Bai

Amphiphilic materials can be used for sample preparation of chromatography or mass spectrometry. Amphiphilic materials with magnetic properties in combination with magnetic suction devices allow for automated sample preparation. However, conventional synthesis methods are cumbersome and not suitable for the mass production of the material. In this study, a micro-suspension polymerization method was developed to synthesize magnetic amphiphilic resin microspheres (MARMs), providing new ideas for the preparation of amphiphilic microspheres. MARMs with particle sizes ranging from 3 to 6 μm were successfully prepared, with BET surface area up to 653.2 m 2 /g. A magnetic solid-phase extraction method based on MARM-5 was developed for the extraction of four glucocorticoids including Cortisone, Hydrocortisone, Cortodoxone, and Corticosterone. This method had a very short adsorption time of 0.5 min and a total extraction time of only 13 min. The limit of detection for the four glucocorticoids ranged from 0.22 to 0.82 ng/L. There was a good linear relationship between sample concentration and peak area in the range of 25∼500 ng/L. Relative recovery of 98 %∼108 % and internal standard normalized matrix effect factors of 95∼114 % were obtained, and the relative standard deviation was between 2.3 % and 6.3 %. The MARMs would be used as excellent solid extraction material for glucocorticoids.

CAS / MDL: 112-80-1
研究领域: 分析化学 · 材料科学 · 药物分析
✓ 已验证 产品关联 DOI PubMed 高影响因子
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Asian Journal of Pharmaceutical Sciences · 2016 ·Vol. 12 ·期 2 ·202-208 · IF 0

Influence of pretreatment of piperazine ferulate on pharmacokinetic parameters of methotrexate in methotrexate-induced renal injury model rats by HPLC-MS

Huiyan Shi,Chenzhi Hou,Liqiang Gu,Zhe Wei,Hang Xing,Meiyu Zhang,Shixiao Wang,Longshan Zhao,Kaishun Bi,Xiaohui Chen

The present study was designed to investigate the influence of the pretreatment of piperazine ferulate on pharmacokinetic parameters of methotrexate in methotrexate-induced renal injury rats. A simple and efficient high performance liquid chromatography coupled with mass spectrometry (HPLC-MS) method was developed to determine methotrexate in rat plasma. Methotrexate and syringic acid (internal standard) were extracted from rat plasma samples by protein precipitation with acetonitrile. The analysis was performed on a CAPCELL PAK C 18 column (150 mm × 4.6 mm, 5 µm) with acetonitrile and 5 mmol/l ammonium acetate aqueous (10:90, v/v ). The linear range was 5.0 × 10 −2 to 100.0 µg/ml for methotrexate. Other parameters were all within the acceptance criteria. The validated method was successfully applied the pharmacokinetic study of methotrexate between two methotrexate treated groups (with and without the pretreatment of piperazine ferulate). Compared with the methotrexate treated alone group, the pharmacokinetic parameters in the methotrexate with the pretreatment of piperazine ferulate group showed significantly lower MRT (0-t) , MRT (0-∞) and T 1/2 . Results suggested that methotrexate can be rapidly eliminated, cleared or metabolized in rat blood, which might be related to the pretreatment of piperazine ferulate. The method provided deeper insights into rational clinical use of methotrexate with the pretreatment of piperazine ferulate on cancer patients with renal dysfunction.

研究领域: 药理学 · 药物代谢 · 肾脏病学 · 肿瘤学 · 临床药学 · 分析化学
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JOURNAL OF ENVIRONMENTAL SCIENCE AND HEALTH PART B-PESTICIDES FOOD CONTAMINANTS AND AGRICULTURAL WASTES · 2021 · IF 1.99

Dissipation and residue analysis of novel nematicide trifluorocide in ginseng and soil using modified QuEChERS method coupled with HPLC-MS/MS

Zhongbei Zhang,Kai Ding,Zhou Lu,Nan Fang,Bo Wang,Zhiguang Hou,Zhongbin Lu

In the present study, an analytical method that combined a modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) method and high-performance liquid chromatography coupled with tandem mass spectrometry was developed to determine trifluorocide in fresh and dried ginseng roots, plants (stems and leaves), and soil. At three spiked levels (0.01, 0.1, and 1.0 mg kg−1), the mean recoveries (n = 15) of trifluorocide from fresh and dried ginseng roots, plants, and soil were in the range of 95.6 − 109.7%, with relative standard deviations less than 10.0%. The limits of quantitation of different matrices were determined to be 0.01 mg kg−1. Dissipation and residue study of trifluorocide was conducted in ginseng cultivation ecosystems in Northeast China. The t1/2 (half-life) of trifluorocide in ginseng fresh roots, plants, and soil were 8.3–13.1 days, 7.4–10.9 days, and 8.8–10.6 days, respectively. The terminal residues of trifluorocide in ginseng fresh roots were less than 0.01 mg kg−1 after 35 days of trifluorocide application. This study could be beneficial in residue analysis and assist in the scientific application of trifluorocide during ginseng cultivation.

CAS / MDL: 64-18-6
研究领域: 植物保护 · 环境科学 · 分析化学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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FOOD CHEMISTRY · 2022 · IF 9.231

Developing a hydroxyl-functionalized magnetic porous organic polymer combined with HPLC-MS/MS for determining 31 amide herbicides in fruit wine

Can Zhang,Shuo Li,Jing Wu,Tengteng Ping,Ling Ma,Ke Wang,Kaoqi Lian

More and more attention has been paid to undesirable chemical contaminants from food raw materials and ingredients. The study aimed to fabricate novel hydroxyl-functionalized magnetic porous organic polymer Fe 3 O 4 @SiO 2 -NH 2 @Ph-POP and explore its use as magnetic adsorbents for magnetic solid-phase extraction (MSPE) for extracting 31 amide herbicides from fruit wine samples prior to high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Several operational parameters were optimized and the as-prepared magnetic polymer displayed favorable extraction efficiency. The method also showed low limits of detection (0.015–1.412 μg·L -1 ) and limits of quantitation (0.049–4.707 μg·L -1 ). Recoveries for all of the herbicides in four different spiked level samples were between 65.06 % and 101.95 % with intra-day and inter-day relative standard deviations less than 9.89 % and 10.54 %, respectively. The proposed MSPE-HPLC-MS/MS method was successfully applied to simultaneously determine 31 amide herbicides in fruit wine.

研究领域: 分析化学 · 食品科学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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Foods · 2023 ·Vol. 12 ·期 15 ·2875 · IF 5.2

Development of Simultaneous Determination Method of Pesticide High Toxic Metabolite 3,4-Dichloroaniline and 3,5 Dichloroaniline in Chives Using HPLC-MS/MS

Yibo Dong,Xiaolong Yao,Wanping Zhang,Xiaomao Wu

3,4-dichloroaniline (3,4-DCA) and 3,5-dichloroaniline (3,5-DCA) are, respectively, the primary metabolites deriving from the breakdown of phenylurea herbicides and dicarboximide fungicides in both soils and plants, whose residues in vegetable products have a heightened concern considering their higher health risks to humans and greater toxicity than the parent compounds in the environment. In this study, a sensitive high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was developed for the simultaneous determination of 3,4-DCA and 3,5-DCA residues in chive products based on the optimization of HPLC-MS/MS chromatographic and mass-spectrometric conditions using the standard substances and the modified QuEChERS preparation technique. The preparation efficiency of 3,4-DCA and 3,5-DCA from chive samples showed that acetonitrile was the best extractant. The combination of the purification agent graphite carbon black + primary secondary amine and the eluting agent acetonitrile + toluene (4:1,v/v) had a satisfactory purification effect. The linear correlation coefficients (R2) were more than 0.996 with the six concentration range of 0.001–1.000 mg/L for 3,4-DCA and 3,5-DCA. The limit of detection and limit of quantitation of this method was 0.6 and 2.0 µg/kg for 3,4-DCA, as well as 1.0 and 3.0 µg/kg for 3,5-DCA, respectively. The matrix effect range of 3,4-DCA and 3,5-DCA in chive tissues was from −9.0% to −2.6% and from −4.4% to 2.3%, respectively. The fortified recovery of 3,4-DCA and 3,5-DCA in chive samples at four spiked levels of 0.001–1.000 mg/kg was 75.3–86.0% and 78.2–98.1%, with the relative standard deviation of 2.1–8.5% and 1.4–11.9%, respectively. The limit of detection (LOD) and limit of quantification (LOQ) of the method were 0.6, 2.0, and 1.0, 3.03 for 4-DCA and 3,5-DCA, respectively. This study highlights that the analytical method established here can efficiently and sensitively detect residues of 3,4-DCA and 3,5-DCA residues for monitoring chive products. The method was successfully applied to 60 batches of actual vegetable samples from different regions.Keywords:3,4-dichloroaniline;3,5-dichloroaniline;simultaneous determination;UPLC-MS/MS;chive

CAS / MDL: 95-76-1 626-43-7
研究领域: 分析化学 · 食品安全 · 环境科学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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CHEMICAL ENGINEERING JOURNAL · 2022 · IF 16.744

Fabrication of aligned carbon nanofiber doped with SnO2-Sb for efficient electrochemical removal of tetracycline

Chengdong Shi,Shuyan Yu,Congju Li

In recent years, tetracycline (TC) has become an emerging refractory antibiotic pollutant due to excessive use and abuse. The aim of this work is to prepare aligned carbon nanofibrous (ACFs) membrane by electrospinning technology and then dope with SnO 2 -Sb to electrocatalytic degrade TC. The in-situ growth of SnO 2 -Sb on the carbon nanofiber surface to fabricate SnO 2 -Sb/ACFs membrane can increase the oxygen evolution reaction potential and improve conductivity. And the SnO 2 -Sb/ACFs membrane was used as the anodic membrane of a flow-through mode electrochemical membrane reactor to remove TC in aqueous solutions. The outstanding degradation performance of SnO 2 -Sb/ACFs membrane on TC was investigated systematically. The results show that the 3-layer SnO 2 -Sb/ACFs-3 membranes can effectively degrade 20 mg/L TC at an applied potential of 2.5 V. Moreover, SnO 2 -Sb/ACFs-3 membrane shows excellent degradation stability after 10 cycles of degradation experiments. For exploring the possible TC degradation pathways, HPLC-MS was used to identify the main intermediates during the electrochemical oxidation process. The anodic membrane electrode prepared in this work puts forward a new idea for the safe and efficient degradation of TC.

研究领域: 环境科学 · 材料科学 · 电化学 · 水处理
✓ 已验证 DOI 高影响因子
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JOURNAL OF SOLID STATE CHEMISTRY · 2021 · IF 3.498

Multifunctional boronic acid-functionalized magnetic nanohybrid: An efficient and selective adsorbent of cis-diol-flavonoids

FuKai Li,Min Wang,Jian Zhou,MengRui Yang,TongTong Wang

A novel magnetically and efficiently multifunctional boronic acid (BA) -functionalized core-shell nanohybrid (Fe 3 O 4 @SiO 2 @BA) was prepared for capture and separation of cis -diol-flavonoids. The morphology and physicochemical properties of resultant nanoparticles were systematically characterized via several techniques, and the results confirmed that the target nanohybrids were successfully functionalized and modified. Meanwhile, two flavonoids (quercetin and luteolin) were selected to investigate the selective capture of the Fe 3 O 4 @SiO 2 @BA in procedure of magnetic solid phase extraction (MSPE). The main parameters influencing the adsorption and elution conditions were systematically investigated and optimized. Furthermore, the adsorption kinetic models were adopted to elucidate the adsorption process , indicating that the pseudo-second-order model was suitable to explain the adsorption kinetics. Under the optimum conditions, the MSPE-HPLC-MS/MS approach was established with a wide linear dynamic range and good linearity (R 2  ​> ​0.999), low limits of detection (0.0096–0.033 ​μg ​L −1 ) and satisfactory recoveries (91–107.6%). The proposed analytical method was successfully applicated by determining the content of target flavonoids in food samples (apple and onion). Accordingly, the prepared nanohybrid could serve as an efficient, rapid and economical potential adsorbent for extracting cis -diol-flavonoids in complex food samples.

研究领域: 纳米技术 · 分析化学 · 食品科学
✓ 已验证 DOI 高影响因子
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