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Frontiers in Environmental Science · 2022 · IF 5.411

The Disappearance Behavior, Residue Distribution, and Risk Assessment of Kresoxim-Methyl in Banana (Musa nana Lour.) Based on a Modified QuEChERS Procedure Using HPLC-MS/MS

Wang Siwei,Sun Haibin,Liu Yanping,Wang Xiaonan,Chang Hong

A modified-QuEChERS method to determine kresoxim-methyl in banana and soil was developed and validated via high-performance liquid chromatography–tandem mass spectrometry (HPLC-MS/MS). The dissipation behavior, residue distribution, and risk assessment of kresoxim-methyl in banana were further investigated based on this method. The dissipation behavior of kresoxim-methyl in banana and soil was described by using first-order kinetics and its half-life, 4.8–5.7 days and 5.5–6.5 days, respectively. The concentrations of kresoxim-methyl were 0.03–0.08 mg kg−1, 0.06–0.17 mg kg−1, and <0.01 mg kg−1 for a whole banana, peel, and pulp, respectively, on the basis of spraying three times the recommended dosage and pre-harvest interval (PHI, 42 days). The results showed that the risk quotient of kresoxim-methyl in banana to people exhibited an acceptable low dietary risk. This current study could help in guiding the scientific and proper usage of this formulation.

CAS / MDL: 64-18-6
研究领域: 农业化学 · 食品科学 · 环境科学
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Analytical Methods · 2016 ·Vol. 8 ·期 6 ·1405-1414 · IF 1.915

Simultaneous determination of rabeprazole enantiomers and their four metabolites after intravenous administration in beagle dogs by a stereoselective HPLC-MS/MS method and its application in pharmacokinetic studies

Na Cao,Lei Liu,Yuan-bin Hao,Li-li Sun,Qiao-gen Zou,Xing-ling Ma,Kai-he Xiong

A sensitive, rapid and stable HPLC-MS/MS method has been developed and validated for the determination of rabeprazole enantiomers and their four metabolites, namely rabeprazole thioether, rabeprazole sulfone and desmethyl rabeprazole enantiomers, in beagle dog plasma using esomeprazole as the internal standard. The analytes and the internal standard were extracted from plasma samples by liquid–liquid extraction and separated on a Chiral-HSA column using acetonitrile-10 mmol L−1 ammonium acetate as the mobile phase by gradient elution. The method was validated with respect to sensitivity, specificity, linearity, precision, accuracy and especially the stability of analytes under various conditions, and was successfully applied in evaluating the pharmacokinetic profiles of racemic rabeprazole, the pure enantiomers and their metabolites in beagle dogs after single intravenous administration of (R)-rabeprazole sodium injection (at 0.33, 1 and 3 mg kg−1), (S)-rabeprazole sodium injection (at 1 mg kg−1) and racemic rabeprazole sodium injection (at 2 mg kg−1). The two enantiomers showed different profiles of pharmacokinetic parameters. The AUC0–t and t1/2 values of (R)-rabeprazole were higher and the clearance (CL) value of (R)-rabeprazole was lower than that of (S)-rabeprazole. Compared to (S)-rabeprazole, the higher absorption and slower elimination of (R)-rabeprazole explain why (R)-rabeprazole is more effective than the racemate.

CAS / MDL: 631-61-8
研究领域: 药物分析 · 药理学 · 临床医学
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MICROCHEMICAL JOURNAL · 2021 · IF 4.821

Cyclodextrin-derivatized hybrid nanocomposites as novel magnetic solid-phase extraction adsorbent for preconcentration of trace fluoroquinolones from water samples coupled with HPLC-MS/MS determination

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

A novel cyclodextrin-derivatized hybrid magnetic nanocomposite, denoted as Fe 3 O 4 @SiO 2 @CD, was fabricated and employed as the adsorbent of magnetic solid-phase extraction (MSPE) for preconcentration of elven fluoroquinolones (FQs) from water samples. The prepared nanoparticles exhibited excellent magnetic responsiveness (56.7 emu g −1 ), uniform size distribution (about 300 nm), good thermal and chemical stability, excellent reusability and superior chemical affinities to the target FQs via hydrogen bond, host–guest inclusion complexation and π–π interactions. Under the optimized conditions, the MSPE was coupled with HPLC-MS/MS to sensitively quantify trance levels of FQs in environmental water. The developed method revealed satisfactory precision with RSDs lower than 4%, good linearity (R 2  ≥ 0.9981), low limits of detection (0.0014–0.023 µg L −1 ) and satisfactory recoveries (93.2–105%). Furthermore, the proposed approach was validated by analyzing the Certified Reference Material of GBW 10152 and GBW 10153 chicken meat powder. These results demonstrated that the Fe 3 O 4 @SiO 2 @CD nanoparticles are a promising magnetic adsorbent for FQs, and the established MSPE-HPLC-MS/MS approach is suitable for simultaneous analysis of trace levels of FQs in actual samples.

研究领域: 分析化学 · 环境科学 · 药物分析
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FOOD CHEMISTRY · 2024 · IF 8.5

Eco-friendly chitosan microspheres as a novel one-step sorbent for the rapid purification and determination of pesticides and veterinary drug multi-residues in aquatic products with HPLC-MS/MS

Ruidong Zhou,Yupeng Wen,Wendi Huo,Cong Kong,Guangxin Yang,Huan Liu,Chaoying Zhang,Yingchun Mu,Dongmei Huang,Jincheng Li

A modified QuEChERS method was developed to determine multi-class pesticide and veterinary residues in aquatic products. Chitosan microspheres were conveniently synthesized and utilized as the cleanup adsorbent in the QuEChERS procedure, showcasing rapid filtration one-step pretreatment ability for the determination of drug multi-residues in aquatic products. Compared to conventional synthetic sorbents, chitosan microspheres not only have good purification performance, but also have renewable and degradable properties. This novel sorbent worked well in the simultaneous determination of 95 pesticides and veterinary drug residues in aquatic products after being combined with an improved one-step vortex oscillating cleanup method. We achieved recoveries ranging from 64.0% to 115.9% for target drugs in shrimp and fish matrix. The limits of detection and quantification were 0.5–1.0 and 1.0–2.0 μg kg −1 , respectively. Notably, hydrocortisone was detected with considerable frequency and concentration in the tested samples, underscoring the necessity for stringent monitoring of this compound in aquatic products.

CAS / MDL: 9012-76-4 64-18-6
研究领域: 分析化学 · 环境科学 · 食品安全
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MICROCHIMICA ACTA · 2018 ·Vol. 185 ·期 3 ·1-9 · IF 5.705

A hollow porous molecularly imprinted polymer as a sorbent for the extraction of 7 macrolide antibiotics prior to their determination by HPLC-MS/MS

Ji Shunli,Li Tengfei,Yang Wen,Shu Chang,Li Duo,Wang Yan,Ding Li

A hollow porous molecularly imprinted polymer (HPMIP) is described for use in dispersive solid phase extraction of macrolide antibiotics (MACs). The HPMIP was prepared by using spiramycin as the template, methacrylic acid as the functional monomer, and mesoporous MCM-41 (Mobile Composition of Matter No. 41; with a size of about 100 nm) as a sacrificial support. The sorbent was characterized by Fourier transform infrared spectrometry, transmission electron microscopy, nitrogen adsorption and thermo-gravimetric analysis. Several parameters affecting the extraction efficiency were optimized. The material has a large surface area (359 m 2 ·g −1 ), and most recognition sites are located on the surface of the HPMIPs. This results in high binding capacity (120 μmol·g −1 ) and fast binding (20 min) in comparison to either MCM-41-core surface MIPs or solid MIPs. The method was applied to the extraction of the MACs azithromycin, spiramycin, tilmicosin, tylosin, clarithromycin, roxithromycin and josamycin from spiked honey. The recoveries, determined by HPLC-MS/MS, ranged from 88.0% to 117% at the three spiking levels tested (1, 5 and 20 μg·kg −1 ). Intra-day and inter-day assay precision at three spiking levels are <10.7% (for n  = 6) and 12.6% ( n  = 3), respectively. The limits of detection are between 3 and 17 ng·kg −1 . This indicates the superiority of the method in selective extraction of macrolides even from complex matrices. Hollow porous molecularly imprinted polymers using spiramycin as the template are shown to be viable dispersive solid phase extraction adsorbents for selective enrichment of macrolide antibiotics in honey products prior to their quantitation by HPLC-MS/MS.

研究领域: 分析化学 · 食品科学
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Journal of Pharmaceutical Analysis · 2020 · IF 2.673

Determination of bioactive components in the fruits of Cercis chinensis Bunge by HPLC-MS/MS and quality evaluation by principal components and hierarchical cluster analyses

Yuan Hong,Xiaoyan Liao,Zilin Chen

The fruits of leguminous plants Cercis Chinensis Bunge are still overlooked although they have been reported to be antioxidative because of the limited information on the phytochemicals of C. chinensis fruits. A simple, rapid and sensitive HPLC-MS/MS method was developed for the identification and quantitation of the major bioactive components in C. chinensis fruits. Eighteen polyphenols were identified, which are first reported in C. chinensis fruits. Moreover, ten components were simultaneously quantified. The validated quantitative method was proved to be sensitive, reproducible and accurate. Then, it was applied to analyze batches of C. chinensis fruits from different phytomorph and areas. The principal components analysis (PCA) realized visualization and reduction of data set dimension while the hierarchical cluster analysis (HCA) indicated that the content of phenolic acids or all ten components might be used to differentiate C. chinensis fruits of different phytomorph.

CAS / MDL: 64-18-6
研究领域: 药用植物学 · 分析化学 · 植物科学
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MICROCHIMICA ACTA · 2023 ·Vol. 190 ·期 10 ·1-13 · IF 5.7

Room-temperature synthesis of imine-linked magnetic covalent organic polymers in deep eutectic solvents for the extraction of flavonoids and their determination with HPLC–MS/MS

Bian Yu,Zhang Yuan,Liu Tong,Zhang Feng,Gao Hui-yuan

A novel imine-linked magnetic covalent organic polymer, Fe 3 O 4 @TAB-TFPT, was synthesized using environmentally friendly deep eutectic solvents as the reaction medium instead of conventional organic solvents. The materials were characterized by scanning electron microscope (SEM), transmission electron microscopy (TEM), FT-IR, N 2 adsorption-desorption isotherms, energy dispersive spectrometer (EDS), X-ray photoelectron spectra (XPS), and thermo gravimetric analysis (TGA). Subsequently, the materials were employed as an adsorbent for magnetic solid-phase extraction (MSPE) of flavonoids, including Kurarinone, Norkurarinone, Xanthohumol, and Isoxanthohumol, prior to their determination by HPLC–MS/MS. The validation results demonstrate good linearity within the concentration range 0.1–1000 ng∙mL −1 ( R 2  ≥ 0.9963), high enrichment factors ranging from 18.9 to 30.7, and low LODs (0.01–0.05 ng∙mL −1 ) and LOQs (0.05–0.1 ng∙mL −1 ). Furthermore, recoveries between 80.60% and 108.40% with relative standard deviations ≤ 8.49% were achieved. The proposed MSPE-HPLC–MS/MS method was successfully applied to the determination of flavonoids in Sophora flavescens Aition sample. Graphical Abstract

CAS / MDL: 108-72-5
研究领域: 分析化学 · 材料科学
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JOURNAL OF HAZARDOUS MATERIALS · 2024 · IF 12.2

High-sensitive determination of tetracycline antibiotics adsorbed on microplastics in mariculture water using pre-COF/monolith composite-based in-tube solid phase microextraction on-line coupled to HPLC-MS/MS

Jinling Pang,Hongzhe Chen,Huige Guo,Kunning Lin,Shuyuan Huang,Beichen Lin,Yuanbiao Zhang

Microplastics (MPs) act as carriers for organic pollutants ( e.g. antibiotics) and microorganisms ( e.g. bacteria) in waters, leading to the proliferation of antibiotic resistance genes. Moreover, the antibiotics adsorbed on MPs may exacerbate this process. For further research, it is necessary to understand the types and amounts of antibiotics adsorbed on MPs. However, due to the heavy work of MPs collection and sample pretreatment, there is a lack of analytical methods and relevant data. In this study, an in-tube solid phase microextraction (IT-SPME) on-line coupled to HPLC-MS/MS method based on amorphous precursor polymer of three-dimensional covalent organic frameworks/monolith-based composite adsorbent was developed, which could efficiently capture, enrich and analyze tetracycline (TCs) antibiotics. Under the optimal extraction parameters, the developed method was capable of detecting TCs at levels as low as 0.48–1.76 pg. This method was applied to analyze the TCs adsorbed on MPs of different particle sizes in mariculture water for the first time, requiring a minimum amount of MPs of only 1 mg. Furthermore, it was observed that there could be an antagonistic relationship between algal biofilm and TCs loaded on MPs. This approach could open up new possibilities for analyzing pollutants on MPs and support deeper research on MPs.

研究领域: 环境科学 · 分析化学
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JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY · 2021 · IF 5.279

Establishment of a HPLC–MS/MS Detection Method for Glyphosate, Glufosinate-Ammonium, and Aminomethyl Phosphoric Acid in Tea and Its Use for Risk Exposure Assessment

Yong Wang,Wanjun Gao,Yeyun Li,Yu Xiao,Wei Song,Ting Yao,Manhuan Cheng,Wenjuan Wang,Ruyan Hou

The tea shrub is grown in long-standing orchards, an environment that is suitable for persistent weed growth, which is increasingly controlled by herbicides. Therefore, there is increasing concern that tea consumers may be exposed to herbicide residues. In this study, the levels of glufosinate-ammonium (GLU), glyphosate [N-(phosphonomethyl) glycine; PMG], and its metabolite aminomethyl phosphoric acid (AMPA) were determined in tea samples by HPLC–MS/MS using several current purification methods and a new method that we developed herein. The matrix effect of our proposed method was between -27.3 and 27.7%, which was lower than that in other methods, indicating that this method effectively reduced the interference of tea matrix in the mass spectrometry process. This method was used to determine the levels of PMG, GLU, and AMPA in 780 samples, including six traditional Chinese teas (green tea, black tea, oolong tea, dark tea, white tea, and yellow tea) and a floral tea, from 14 provinces of China. Probability estimates showed that the 95th percentile risk entropy values of the three pesticide residues were far below the acceptable risk level. The risk assessment results showed that exposure to PMG, GLU, and AMPA caused by drinking tea beverages poses no significant risk to human health.

CAS / MDL: 631-61-8
研究领域: 分析化学 · 环境科学 · 食品安全
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MICROCHEMICAL JOURNAL · 2024 · IF 4.9

Discovery of COX-2 and 5-LOX dual targeted inhibitors from Nauclea officinalis by employing a combination of affinity ultrafiltration and HPLC-MS/MS

Guanghou Wang,Xueqian Tang,Feixu Qin,Hongjin Wang,Hao Zhang,Hanyue Li,Lan Wei,Lixin Sun

Nauclea officinalis ( N. officinalis ), a medicinal plant of the genus Nauclea in the Rubiaceae family, is used to treat bronchitis, pneumonia and acute tonsillitis and enteritis in China. Extracts of N. officinalis include more than 60 alkaloids, which exert all kinds of pharmacological effects, such as antiproliferative, antiparasitic, antimicrobial, anticancer, and anti-inflammatory activities. In this study, an affinity ultrafiltration and high-performance liquid chromatography- tandem mass spectrometry (AUF-LC-MS/MS) approach was constructed and validated, and was applied to rapidly screen COX-2/5-LOX inhibitors in N. officinalis extracts (NOE). To gain a more comprehensive and profound understanding of the anti-inflammatory mechanism of N. officinalis . Central Composite Design (CCD) of Response Surface Method (RSM) was used to optimize extraction conditions for potential COX-2/5-LOX inhibitors from NOE. Next, COX-2/5-LOX dual targeted inhibitors were screened from NOE using AUF-LC-MS/MS, and the biological activity of the screened ligands was demonstrated by enzyme inhibition assay. Finally, the preferred binding modes for these COX-2/5-LOX inhibitors were then determined by molecular docking, and compared with active drugs celecoxib and zileuton, respectively, to further explore ligand active binding sites and intersections between ligands and target proteins. The optimum extraction conditions were follows: ethanol concentration of 79 %, liquid − solid ratio of 11.8 v / w and extraction time of 1.8 h. The results of COX-2 inhibition assay showed that angustine (AU) had the more stronger inhibition activity with an IC 50 of 20.49 μM, followed with IC 50 of angustidine (AD) and nauclefine (NF) were 35.89 and 60.45 μM, respectively. Among the three components, AU also exhibited the highest inhibition of 5-LOX with an IC 50 of 1.18 μM, followed by NF and AD at 2.75 and 4.35 μM, respectively. Owing to the synergistic effect of multiple components make NOE exhibit strong inhibitory activity, it is shown potent inhibitory activities with an IC 50 at 9.47 and 6.16 μg/mL for COX-2 and 5-LOX, respectively. This work has demonstrated that NF, AD, and AU are potential COX-2/5-LOX dual-target inhibitors, indicating that N. officinalis anti-inflammatory activities were partially based on these COX-2/5-LOX inhibitors. These research results can also be further used for developed or improved anti-inflammatory agents with more beneficial effects.

CAS / MDL: 506-32-1 111406-87-2
研究领域: 药理学 · 药物化学 · 植物科学 · 分析化学
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Journal of Pharmaceutical Analysis · 2020 · IF 2.673

Identification and quantification of the bioactive components in Osmanthus fragrans roots by HPLC-MS/MS

Xiaoyan Liao,Yuan Hong,Zilin Chen

The roots of O. fragrans are also a valuable resource in addition to its flowers and fruits. In this study, the HPLC-MS/MS method used for analyzing the chemical constituents in O. fragrans roots extract was developed, which showed high sensitivity for both qualitative and quantitative analyses. Thirty-two compounds were first discovered in O. fragrans roots, one compound of which was reported for the first time. The simultaneous determination method for acteoside, isoacteoside, oleuropein and phillyrin was validated to be sensitive and accurate. Then it was applied to determine the content of bioactive components in O. fragrans roots from different cultivars. The content of oleuropein and phillyrin in the twelve batches was relatively stable, while the content of acteoside and isoacteoside varied greatly. Moreover, the therapeutic material basis and mechanism of O. fragrans roots exerting its traditional pharmacodynamics were analyzed by network pharmacology. The results showed that O. fragrans roots might be effective for the treatment of inflammation, cardiovascular diseases, cancer, and rheumatoid arthritis, which is consistent with the traditional pharmacodynamics of O. fragrans roots. This work can provide an analytical method for the comprehensive development of O. fragrans roots.

CAS / MDL: 64-18-6
研究领域: 药理学 · 分析化学 · 中医药学 · 植物科学
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Journal of Analytical Methods in Chemistry · 2022 · IF 2.594

Measurement of Pharmacokinetics and Tissue Distribution of Four Compounds from Nauclea officinalis in Rat Plasma and Tissues through HPLC-MS/MS

Yuhuang Wu,Liyan Li,Guxu Ming,Xinyue Ma,Changfu Liang,Yonghui Li,Xiaoning He

A rapid, sensitive, selective, and accurate HPLC–MS/MS method was developed and validated for the simultaneous determination of chlorogenic acid, naucleactonin C, khaephuoside A 3,4-dimethoxyphenyl-1-O-β-apiofuroseyl(1 ⟶ 2)-β-D-glucopyranoside in rat plasma and tissues after oral administration of Nauclea officinalis extracts. Chloramphenicol was used as an internal standard (IS). The plasma and tissue samples were extracted by protein precipitation with methanol-ethyl acetate (1 : 1, v/v) including 0.1% (v/v) formic acid. The chromatographic separation was achieved by using an C18 column with gradient elution using mobile phase, which consisted of 0.1% formic acid water (A) and acetonitrile (B) and the flow rate of 0.8 mL/min. Mass spectrometric detection was performed in multiple reaction monitoring (MRM) mode utilizing electrospray ionization (ESI) in negative mode. The developed method exhibited good linearity (determination coefficients, R2 ≥ 0.9849), and the lower limits of quantification were 2, 5, 5, and 25 ng/mL for chlorogenic acid, naucleactonin C, khaephuoside A, and 3,4-dimethoxyphenyl-1-O-β-apiofuroseyl(1 ⟶ 2)-β-D-glucopyranoside. The intraday and interday precisions (relative standard deviation, RSD) were less than 12.65%, while the accuracy was ranged from 86.31 to 114.17%. The recovery rate were 51.85–97.06%, 75.99–106.68%, 77.46–105.35%, and 68.36–103.75% for chlorogenic acid, naucleactonin C, khaephuoside A, and 3,4-dimethoxyphenyl-1-O-β-apiofuroseyl(1 ⟶ 2)-β-D-glucopyranoside the matrix effects were 50.17–116.62%, 86.75–115.99%, 45.79–87.44%, and 51.60–92.34% for chlorogenic acid, naucleactonin C, khaephuoside A, and 3,4-dimethoxyphenyl-1-O-β-apiofuroseyl(1 ⟶ 2)-β-D-glucopyranoside in different matrix. The developed method was successfully applied to a pharmacokinetic study and tissue distribution of four compounds in rats after oral administration of Nauclea officinalis extracts.

CAS / MDL: 141-78-6 64-18-6
研究领域: 药理学 · 分析化学 · 中药学
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