MICROCHEMICAL JOURNAL
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2025
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IF 5.1
Wanxin Zhang,Yujie Chen,Zhe Song,Zhonghui Zhang,Bo Wu,Bin Di,Mengxiang Su
Synthetic cannabinoids (SCs) are new psychoactive substances with an increasingly large number of users and strong addictive properties. The metabolites produced after smoking SCs flow into sewage with urine and feces. Owing to the extremely low concentration of SCs and the complexity of sewage matrix, the development of different adsorbent materials to enrich SCs in sewage and enhance detection sensitivity is essential. However, existing adsorption materials, such as spherical magnetic solid-phase extraction (MSPE) materials, possess drawbacks of easily saturated functional sites, long extraction time, and low sensitivity. To solve these problems, we proposed two novel poly (glycerol methacrylate- co -trimethylolpropane trimethacrylate)/poly (dopamine- co -chitosan)-functionalized magnetic carboxylated multiwalled carbon nanotubes (GTMC/DCMC) as adsorbents and developed two highly sensitive quantitative analytical techniques to detect eleven SCs in wastewater. The magnetic adsorbents were fully characterized using transmission electron microscopy, infrared spectroscopy, vibrating sample magnetometry, and X-ray photoelectron spectroscopy. Additionally, two MSPE-UPLC-MS/MS methods were developed and validated to determine eleven trace analytes in wastewater. The validation results show that the limits of quantification (LOQ) of GTMC is 5.0 ng/L and the LOQ of DCMC is 2.5 ng/L. Additionally, the recoveries of GTMC range from 63.17 % to 86.22 %, and the recoveries of DCMC range from 61.29 % to 97.41 %. The relative standard deviations of intraday and interday precision are less than 10 %. The MSPE-UPLC-MS/MS methods are successfully applied to real wastewater samples, and the entire pretreatment process is completed in 25 min. Therefore, the proposed methods are convenient, rapid, sensitive, and reliable for the determination of trace SCs in wastewater.
研究领域:
环境分析化学
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药物代谢
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毒理学
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环境污染监测
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分子探针与检测技术
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BMC Chemistry
·
2025
·Vol. 19
·期 1
·194
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IF 4.6
Chenjian Zhou,Peiqi Wang,Jie Chen,Hualu Wu,Yige Yu
Parsaclisib is a novel, potent, highly selective, next-generation oral inhibitor of phosphatidylinositol 3-kinase δ (PI3Kδ) for patients with relapsed or refractory B-cell malignancies. However, there is no accurate and rapid method for the determination of parsaclisib. The aim of this study was to establish a rapid, specific and reliable ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) method for the determination of parsaclisib, and to investigate in vitro metabolic stability using rat liver microsomes (RLMs) and in vivo pharmacokinetics in rats. Parsaclisib was detected by gradient elution on an Acquity UPLC BEH C18 column (2.1 mm × 50 mm, 1.7 μm) using acetonitrile and 0.1% formic acid as mobile phases, and pilaralisib was used as an internal standard (IS). Selective reaction monitoring (SRM) was used for detection. The method showed acceptable intra- and inter-day precision (< 8.6%) and accuracy (2.0–14.9%). The stability of the test samples was reliable during the analysis. In addition, the recoveries and matrix effects of the samples were within acceptable limits and were stable during storage and determination in rat plasma. The pharmacokinetic trend of parsaclisib in rats was also investigated by this newly developed assay after gavage administration of 2.0 mg/kg parsaclisib. Finally, i n vitro results showed that parsaclisib had a slow intrinsic clearance (Clint) value of 2.4 µL/min/mg protein with a half-life (t 1/2 ) value of 571.3 min. These findings theoretically supported the potential metabolism of parsaclisib in vivo.
研究领域:
药物分析
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药代动力学
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药物代谢
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分析化学
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肿瘤学
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生物分析方法开发
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Foods
·
2025
·Vol. 14
·期 14
·2421
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IF 5.1
Mengqiong Yang,Guangming Mei,Daoxiang Huang,Xiaojun Zhang,Pengfei He,Si Chen
A sensitive method was developed for detecting diazepam residues in aquatic products using magnetic dispersive solid-phase extraction (MDSPE) coupled with ultra-performance liquid chromatography–tandem mass spectrometry (UPLC-MS/MS). Samples extracted with 1% ammonia–acetonitrile were purified using synthesized Fe3O4@SiO2-PSA nanoparticles via MDSPE before UPLC-MS/MS analysis. Separation was performed on a C18column with gradient elution using 0.1% formic acid–2 mM ammonium acetate/methanol. Detection employed positive electrospray ionization (ESI+) in multiple reaction monitoring (MRM) mode. Characterization confirmed Fe3O4@SiO2-PSA’s mesoporous structure with excellent adsorption capacity and magnetic properties. The method showed good linearity (0.1–10 μg/L,r> 0.99) with an LOD and LOQ of 0.20 μg/kg and 0.50 μg/kg, respectively. Recoveries at 0.5–15.0 µg/kg spiking levels were 74.9–109% (RSDs 1.24–11.6%). This approach provides rapid, accurate, and high-precision analysis of diazepam in aquatic products, meeting regulatory requirements.
研究领域:
分析化学
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食品安全
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材料科学
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Journal of Analytical Methods in Chemistry
·
2026
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IF 2.1
Mengyue Zhang,Feng Han,Mingxuan Yang,Zhishan Ye,Ying Cui,Yuefei Wang,Jing Yang,Xin Chai
Fuganlin oral liquid (FOL) has been clinically employed for the treatment of pediatric qi deficiency colds, manifesting symptoms such as fever, cough, asthma, and sore throat. However, the chemical composition and bioactive components of FOL have not been clearly elucidated. In this study, a comprehensive qualitative analysis of FOL was conducted utilizing ultra‐high‐performance liquid chromatography coupled with quadrupole time‐of‐flight mass spectrometry in conjunction with network pharmacology. A total of 124 chemical components were tentatively characterized, comprising flavonoids, phenolic acids, saponins, coumarins, and others. Among these, 43 compounds were unequivocally identified by comparison with authentic reference standards. Furthermore, network pharmacology analysis revealed that the ingredients of FOL exhibited anti‐inflammatory properties and demonstrated potential efficacy in relieving cough and asthma associated with respiratory tract infections. Collectively, this study provides the first comprehensive characterization of the chemical composition in FOL and explores the potential pharmacological mechanisms of its bioactive constituents, thereby providing scientific support for quality control standards and clinical applications.
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JOURNAL OF CHROMATOGRAPHY A
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2026
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IF 4
Baocheng Ji,Yanxin Wang,Li Ma,Mengwei Zhang,Yumeng Liu,Xu Xu,Junguang Li,Ke Li,Dianbo Zhao,Yanhong Bai
A rapid, convenient, and efficient dispersive solid-phase extraction approach, integrating ultraperformance liquid chromatography–tandem mass spectrometry and pretreated pine pollen, was developed for sensitive quantification of 13 heterocyclic amines (HCAs) in sesame oil. Critical parameters, namely sorbent type and dosage, adsorption mode and duration, detergent dosage, eluent additive and volume, and elution cycles, were systematically optimized to evaluate their effects on the HCA recovery. The proposed method was verified for all the 13 HCAs, demonstrating favorable analytical characteristics with remarkable linear relationships (coefficient of determination, R 2 ≥ 0.998), adequate recoveries (64.2%–99.4%), acceptable intra- and inter-day precision (relative standard deviations ≤ 10.4%), and low limits of detection (0.02–0.83 μg/kg) and quantification (0.07–2.70 μg/kg). The proposed approach offers distinct advantages, including rapidity, simplicity, cost-effectiveness, and minimized organic solvent consumption, demonstrating great potential for accurately analyzing HCAs in complex food matrices.
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BMC Pharmacology & Toxicology
·
2025
·Vol. 26
·期 1
·200
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IF 2.7
Chen Xiaohai,Chen Dongxin,Wu Hualu,Xia Hailun,Lan Tian,Xu Ren-ai
This study aimed to develop and validate a novel ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) method for the simultaneous determination of iloperidone (ILP) and its metabolites P88, P95 in rat plasma and to investigate drug-drug interaction (DDI) between shikonin and ILP in Sprague-Dawley rats. The separation of the analytes was performed on a UPLC BEH C18 column in the mobile phase (acetonitrile and water with 0.1% formic acid) with the flow rate of 0.4 mL/min. The quantitative analysis was performed in positive ion mode. A total of 10 Sprague-Dawley rats were divided into two groups: control group (1.0 mg/kg ILP alone) and experimental group (20 mg/kg shikonin plus 1.0 mg/kg ILP) to investigate the influence of shikonin on ILP metabolism in rats. We successfully established a quick UPLC-MS/MS analytical method for simultaneously detecting ILP and its two metabolites in rat plasma. Linearity, matrix effect, recovery, accuracy, precision and stability of this quantitative method was satisfied with Food and Drug Administration (FDA) guidelines. In addition, in vitro studies demonstrated that shikonin significantly inhibited CYP3A4- and CYP2D6-mediated metabolism in both rat liver microsomes (RLM) and human liver microsomes (HLM). Furthermore, we found the main pharmacokinetic parameters of ILP, such as AUC (0−t) and the peak plasma concentration (C max ), were obviously changed, which were about twice higher in experimental group than the values in control group. The data demonstrated that shikonin obviously changed the main pharmacokinetics of ILP and its metabolites in rats. In the future clinical use, we should pay more attention to the concomitant application of shikonin and ILP in humans.
研究领域:
药物分析
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药代动力学
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药物代谢
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分析化学
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毒理学
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MOLECULES
·
2023
·Vol. 28
·期 5
·2022
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IF 4.6
Ting Zhang,Dingrong Wan,Yuanyuan Li,Sisi Wang,Xiuteng Zhou,Fatemeh Sefidkon,Xinzhou Yang
TheArtemisia argyiLévl. et Van. growing in the surrounding areas of Qichun County in China are called Qiai (QA). Qiai is a crop that can be used both as food and in traditional folk medicine. However, detailed qualitative and quantitative analyses of its compounds remain scarce. The process of identifying chemical structures in complex natural products can be streamlined by combining UPLC-Q-TOF/MS data with the UNIFI information management platform and its embedded Traditional Medicine Library. For the first time, 68 compounds in QA were reported by the method in this study. The method of simultaneous quantification of 14 active components in QA using UPLC-TQ-MS/MS was reported for the first time. Following a screening of the activity of QA 70% methanol total extract and its three fractions (petroleum ether, ethyl acetate, and water), it was discovered that the ethyl acetate fraction enriched with flavonoids such as eupatilin and jaceosidin had the strongest anti-inflammatory activity, while the water fraction enriched with chlorogenic acid derivatives such as 3,5-di-O-caffeoylquinic acid had the strongest antioxidant and antibacterial activity. The results provided the theoretical basis for the use of QA in the food and pharmaceutical industries.Keywords:Artemisia argyiLévl. et Van.;UPLC-MS;quantification;anti-inflammatory;antioxidant
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SCIENTIA HORTICULTURAE
·
2023
·
IF 4.3
Muhammad Khalid Hameed,Wajid Umar,Ali Razzaq,Shiwei Wei,Qingliang Niu,Danfeng Huang,Liying Chang
Lettuce is an important leafy vegetable and an excellent source of phytochemicals in human diets. However, the metabolic levels in different green and red type lettuce varieties are not fully explored. Therefore, it is important to explore and identify the selected health promoting secondary metabolites in green and red type lettuce varieties with having different phenotypic characteristics. In this study, we explored the selected secondary metabolites, total polyphenol, antioxidants activities, total flavonoids and anthocyanin contents in 32 lettuce varieties of green and red color. The results showed that green and red type lettuce varieties showed a significant difference in lactupicrin, chlorogenic acid, caffeoylmalic acid, syringic acid and quercetin 3-D-galactoside. Selected metabolites showed a significant variation in green and red type lettuce varieties depends upon different color and phenotypic characteristics. Total flavonoids and anthocyanin contents were found more in red type lettuce varieties while the total polyphenols and total antioxidants were found significantly higher in green type lettuce varieties. Tentative identified 78 metabolites with online databases, the published literature and standards including phenolic acid, flavonoids and glycosylated flavonoids. The metabolomic profiling was present at significantly difference in green and red type lettuce varieties which suggested the significant variation between green and red type lettuce varieties to secondary metabolism. This study provides a selection of lettuce varieties for further studies on the basis of color and phenotypic characteristics for improving the nutritional value, quality and yield of lettuce.
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INTERNATIONAL JOURNAL OF BIOLOGICAL MACROMOLECULES
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2023
·
IF 8.2
Peiyi Jin,Linzhou Chen,Jinjian Zhong,Tiefeng Yuan,Lin Gan,Jilong Huang,Liping Wang,Huajun Fan,Chen Lin
Dioscoreae nipponica Makino ( D. nipponica ) as the rhizome of dioscoreaceae rich in steroidal saponins, has been reported to have the hypolipidemic effects etc. However, it is still unclear which exact active components are primary responsible for the beneficial effects. This study was conducted to fish out the lipase inhibitors from D. nipponica , and evaluate the inhibitory activity on porcine pancreatic lipase (PPL) through in vitro kinetic assay using p -nitrophenyl palmitate as substrate. Accordingly, the ethanolic extract was subjected to D101 macroporous resin purification for spectrophotometric screening, high performance liquid chromatography (HPLC) separation and structural characterization by ultra-performance liquid chromatography-quadrupole time-of-flight mass spectrometry. Through orlistat validation, the PPL inhibitory activity and IC 50 value of the extract were respectively 68.34 ± 1.47 % and 107.05 μg/mL under the optimized inhibition conditions. From 6 steroidal saponins identified, the inhibitory components named the protodioscin, protogracillin, dioscin and gracillin were fished out by grouping separation and HPLC analysis. Furthermore, dioscin and gracillin with the parent structure of diogenin were confirmed as the major inhibitors by virtue of stability tests based on transformation of protodioscin and protogracillin. Finally, the inhibitory mechanism of the major inhibitors toward PPL was further clarified by kinetic analysis and molecular docking analysis. The proposed method not only revealed the PPL inhibitory components in D. nipponica , but also provided an effective approach to hierarchical screening of PPL inhibitors from natural plants.
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Frontiers in Chemistry
·
2022
·
IF 5.545
Shen Qing,Wang Haixing,Quan Bin,Sun Xiuhua,Wu Guohua,Huang Darong,Wang Qingcheng,Luo Pei
Salvia miltiorrhiza Bunge (SMB) has unambiguous biological functions in cardiovascular diseases, thus has been processed into different medicine forms. However, universal analytical method for fast quantification of bioactive compounds in SMB and SMB derived products is still missing. In this study, a polarity switching strategy was developed and optimized, which enabled the detection of the target compound in both positive and negative ion modes in a single run. The MS2 features of each compound were characterized to select the most prominent transitions for quantitative and qualitative analysis. Afterwards, the performance of this method was validated in terms of linearity (≥0.9916), limit of detection (LOD, 0.003–0.135 ngml−1), limit of quantification (LOQ, 0.010–0.450 ngml−1), precision (48.23 ± 2.58 ngml−1 to 53.72 ± 3.11 ngml−1), recovery (RSD 2.04%–5.79%), and stability (RSD ≤7.52%). Finally, the bioactive compounds in SMB and SMB derived products were determined, among which salvianate A, salvianolic acid A, and rosmarinic acid were the main components in all samples. In conclusion, the polarity switching UPLC-MS/MS method is efficient in accurate determining the bioactive compounds, which greatly shorten the time for analysis when compared with conventional methods. It has great potential quality control of SMB and SMB derived products.
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Toxins
·
2023
·Vol. 15
·期 5
·337
·
IF 4.2
Baoxia Ni,Jin Ye,Zhihong Xuan,Li Li,Xiangrui Wen,Zongwang Li,Hongmei Liu,Songxue Wang
Sample pretreatment is a vital step in the detection of mycotoxins, and traditional pretreatment methods are time-consuming, labor-intensive and generate much organic waste liquid. In this work, an automatic, high-throughput and environmentally friendly pretreatment method is proposed. Immunomagnetic beads technology and dispersive liquid–liquid microextraction technology are combined, and the zearalenone in corn oils is directly purified and concentrated under the solubilization effects of surfactant. The proposed pretreatment method allows for the batch pretreatment of samples without pre-extraction using organic reagents, and almost no organic waste liquid is produced. Coupled with UPLC-FLD, an effective and accurate quantitative detection method for zearalenone is established. The recovery of spiked zearalenone in corn oils at different concentrations ranges from 85.7 to 89.0%, and the relative standard deviation is below 2.9%. The proposed pretreatment method overcomes the shortcomings of traditional pretreatment methods and has broad application prospects.Keywords:immunomagnetic beads;dispersive liquid liquid microextraction;pretreatment;zearalenone;corn oils;UPLC-FLDKey Contribution:An automatic and eco-friendly pretreatment method of zearalenone (ZEN) in corn oils was developed based on immunomagnetic beads with dispersive liquid–liquid microextraction technology. The proposed pretreatment method, coupled with UPLC-FLD, met the accuracy and sensitivity detection requirements of ZEN in corn oils.
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AQUACULTURE INTERNATIONAL
·
2023
·
IF 2.9
Hong Yawen,Pan Yunyun,Zhu Qijian,Li Yongyong,Yang Huicheng,Lin Bangchu,Dong Zheyun,Lou Yongjiang,Fu Shiqian
Due to high-density farming methods and poor farming environments, freshwater fish often have poor muscle texture and a fishy odor before marketing, which impacts consumer acceptance. Short-term low-salinity seawater treatment of freshwater fish before marketing has been found to improve the quality of the fish, but the mechanisms underlying this phenomenon have not yet been revealed. In this study, metabolomics technique was used based on gas chromatography-mass spectrometry (GC–MS) and ultra-performance liquid chromatography-mass spectrometry (UPLC-MS) to screen different metabolites and predict potential metabolic pathways after treatment with low-salinity seawater. The results showed that 3838 metabolites were presented in all of the carp samples, while 62 and 64 differential metabolites were found in the comparative groups (FW, SW, and CK represented freshwater, seawater and non-transient group, respectively). Additionally, 25 and 26 metabolic pathways were enriched from these groups. Glutaric acid, PC, and creatinine might be potential biomarkers. Seawater aquaculture significantly altered the lipid metabolism, nucleotide metabolism, and amino acid metabolism of carp, enhancing its freshness and having a significant impact on its quality. This study provided insights into the metabolic changes in carp under different rearing conditions and also served as a theoretical basis for salinity treatment before freshwater fish are brought to the market.
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危险品化学品经营许可证（带存储）