JOURNAL OF HAZARDOUS MATERIALS
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2025
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IF 11.3
Lingxuan Ma,Fan Nie,Sheng Gong,Yudi Wang,Di Chen,Zijian Wang,Peng Li,Jinchao Wei
Plant growth regulators (PGRs) are extensively deployed in medicinal and edible plants (MEPs) to enhance yields, yet their environmental persistence and potential ecotoxicological effects have raised significant public health concerns. However, current regulatory frameworks remain deficient in PGR-specific residue limits and cross-matrix surveillance tools. Herein, a data modeling-driven broad-spectrum analytical platform was engineered for comprehensive occurrence mapping and dietary exposure assessment of PGRs. Global optimization was achieved through simplex lattice mixture design combined with Derringer’s desirability function, enabling all-inclusive mixed-mode solid-phase extraction (MMSPE) for 64 PGRs (Log K ow −3.80–5.68) across diverse polarity/ionization domains. Integrated with ultra-performance liquid chromatography-triple quadrupole-tandem mass spectrometry (UPLC-QqQ-MS/MS), the MMSPE-UPLC-MS/MS platform facilitated rapid quantification of multi-class PGRs (auxins, cytokinins, gibberellins, brassinosteroids, and growth retardants) in seven MEP matrices. Limits of quantification ranged from 0.016 to 14.392 μg/kg, with average recoveries of 68.93%–118.07% and relative standard deviations of 0.47%–12.88%. Among 140 commercial samples, 30 PGRs were detected (0.07–6392.80 μg/kg), revealing pervasive cross‑matrix contamination and elevated environmental exposure of both endogenous hormones and several synthetic PGRs. Hazard quotient/index-based risk assessments indicated generally acceptable population‑level exposure risk, but highlighted matrix‑dependent risk drivers, with tebuconazole, diuron and paclobutrazol dominating cumulative exposure in specific MEPs. Collectively, this work provided a powerful panoramic screening tool for uncovering cryptic chemical burden in complex herbal matrices, thereby establishing a scientific foundation for prioritizing control lists and refining toxicological benchmarks.
研究领域:
分析化学
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环境科学
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食品安全
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药学
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毒理学
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农业化学
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公共卫生
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DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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2025
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IF 3.1
Xiao-han Peng,Yan-lin Zhao,Zhong Huang,Xin-feng Xia,Kun Wang,Peng Jin,Yan Du,Dao-quan Tang
Currently, treatment with antiepileptic drugs (AEDs) is still the first choice for epileptic patients, while monitoring their blood concentrations is undoubtedly beneficial for minimizing their adverse side effects and optimizing their therapeutic effects. In this study, an ultra-high performance liquid chromatography coupled with tandem mass spectrometry with polarity switching was developed and validated for simultaneous determination of 14 AEDs and 2 active metabolites in human serum. Olanzapine was selected as the internal standard. One-step protein precipitation using methanol containing 0.05 % formic acid was used to treat sample, and the supernatant was injected for analysis without further evaporation and reconstitution. Chromatographic separation was performed on an Aglient Zorbax Eclipse Plus C18 (50 mm × 2.1 mm, 1.8 μm) column with gradient methanol and 0.1 % formic acid in water as mobile phase. Multi-reaction monitoring was performed for quantification of 16 analytes in polarity switching mode. Matrix-matched calibration curves of 16 analytes presented good linearity within the test concentration range ( r > 0.99). The intra- and inter-run accuracies and precisions at the lower limit of quantification, and low, medium and high quality control levels were all less than 20 % or 15 %, respectively. The extraction recovery, matrix effect, and stability were all acceptable under detected conditions. Finally, this method was successfully applied in the quantitation of target analytes in the serum of patients received AEDs.
研究领域:
药理学
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临床医学
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分析化学
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PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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2026
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IF 3.1
Meichen Liu,Yalin Yu,Yifei Jing,Yingxia Guo,Chuya Wang,Hongyu Xue,Hong Liu,Lei Yin,Meiyun Shi
While polyethylene glycol (PEG) is an extensively utilized pharmaceutical polymer with established biocompatibility and regulatory acceptance, the in vivo pharmacokinetics of its bifunctional derivatives, such as α,ω-dipropionic acid polyethylene glycol (PA-PEG-PA), remain largely unexplored. This study presents the development and validation of a highly sensitive and selective UPLC-MS/MS method for the accurate quantification of PA-PEG 12 -PA in various biological matrices, utilizing a straightforward protein precipitation protocol. After intravenous administration in rats (10 mg/kg), PA-PEG 12 -PA demonstrated rapid clearance (t 1/2 = 3.99 ± 1.06 h). Tissue distribution analysis revealed a pronounced affinity for renal accumulation, with kidney concentrations (16473 ± 881 ng/g at 2 h) substantially surpassing those in the liver and lungs, followed by rapid depletion within 24 h. Excretion studies indicated renal clearance as the dominant pathway, with 55.93 % of the administered dose recovered unchanged in urine over 72 h, while fecal excretion was minimal (1.76 %). This work provides the first comprehensive pharmacokinetic and biodistribution profile of PA-PEG 12 -PA, underscoring its renal-driven clearance and tissue disposition. The findings offer crucial insights for the rational design of PEGylated drug delivery systems, and the robust UPLC-MS/MS assay established herein serves as a valuable tool for characterizing polymeric excipients in biological environments.
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MICROCHEMICAL JOURNAL
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2026
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IF 5.1
Shi Wang,Wen-xin Zheng,Zhi-ming Xiao,De-cheng Suo,Jian-chun Xie,Run-xian Li,Yu-chao Feng,Xia Fan
β 2 -agonists are a class of synthetic phenethanolamine compounds that pose multiple risks to public health. In this study, a dual-template magnetic molecularly imprinted polymer (Dual-T Fe₃O₄@MIP) approach was developed to enable the simultaneous detection of 33 β₂-agonists in swine urine and muscle tissues, with preliminary validation of its applicability in complex biological matrices. Briefly, samples were sheared and homogenized, followed by enzymatic hydrolysis using β-glucoronidase/arysulfatase in ammonium acetate buffer at 55 °C for 4 h. Thereafter, β 2 -agonists in the hydrolysate were extracted with the Dual-T Fe 3 O 4 @MIPs and eluted with an acidic methanol solution. The target compounds were quantified by UPLC-MS/MS equipped with an HSS T3 column (100 mm × 2.1 mm, 1.8 μm). The method was further validated in urine and muscle samples, demonstrating excellent linearity (R 2 ≥ 0.9944), high sensitivity (limit of detection ranging from 0.010 to 0.034 μg/kg, limit of quantitation ranging from 0.024 to 0.100 μg/kg), satisfactory recovery (ranging from 82.1% to 107%), and good precision (≤9.1%). Compared with the conventional solid-phase extraction method, which requires 3 h, the proposed method achieved purification in less than 30 min, representing a substantial improvement in analytical efficiency. The proposed approach is reliable, rapid, and user-friendly, making it suitable for routine analytical applications.
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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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2020
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IF 3.209
Authors: Kan Wang,Ting Geng,Wei Jiang,Qiao Zhang,Yi Zhang,Pei-dong Chen,Ming-qiu Shan,Min Zhang,Yu-ping Tang,An-wei Ding,Li Zhang
Rubiae Radix et Rhizoma (called “Qiancao”, QC), the root and rhizome of Rubia cordifolia L., has been widely used in clinical practice for its excellent performance in removing blood stasis and haemostasis. However, after carbonization processing, significant changes occurred in chemical components of the charcoal of Rubiae Radix et Rhizoma (called “Qiancaotan”, QCT), which enhanced the performance in haemostasis and weakened the performance in removing blood stasis in clinic. In order to study the material basis of function variation during processing, a rapid, reliable, accurate and validated UPLC–MS/MS approach was established to determine twelve quinones in QC and QCT simultaneously. Meanwhile, the antithrombotic effect of target components on zebrafish thrombus model induced by phenylhydrazine (PHZ) was investigated. Chromatographic separation was accomplished on an ACQUITY UPLC C 18 column with acetonitrile–water containing 0.2 % (v/v) formic acid as mobile phase, at a flow rate of 0.30 mL/min. Quantitation was performed using multiple reaction monitoring (MRM) in positive and negative ion electrospray ionization (ESI). Furthermore, the activity evaluation studies showed that the reduction of removing blood stasis effect of QCT was due to the decrease of dehydro- α -lapachone, lapachol, rubioncolin C and mollugin. This study demonstrated that the method has been successfully applied to determine the content of twelve quinones responsible for the function variation of QCT, and provided a new insight into the material basis and the effect of eliminating stasis before and after processing of QC.
研究领域:
药理学
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分析化学
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中医药
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PubMed
高影响因子
BMC Pharmacology & Toxicology
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2024
·Vol. 25
·期 1
·1-15
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IF 2.8
Wang Tianyan,Tao Ting,Liu Yi,Dong Jie,Ni Shanhong,Liu Yun,Li Yanli,Xu Ning,Sun Zengxian
Background and purposes It is unclear whether the parent Saxagliptin (SAX) in vivo is the same as that in vitro, which is twice that of 5-hydroxy Saxagliptin (5-OH SAX). This study is to construct a Pharmacokinetic-Pharmacodynamic (PK-PD) link model to evaluate the genuine relationship between the concentration of parent SAX in vivo and the effect. Methods First, we established a reliable Ultra Performance Liquid Chromatography-Mass Spectrometry (UPLC-MS/MS) method and DPP-4 inhibition ratio determination method. Then, the T2DM rats were randomly divided into four groups, intravenous injection of 5-OH SAX (0.5 mg/kg) and saline group, intragastric administration of SAX (10 mg/kg) and Sodium carboxymethyl cellulose (CMC-Na) group. Plasma samples were collected at different time points for subsequent testing. Finally, we used the measured concentrations and inhibition ratios to construct a PK-PD link model for 5-OH SAX and parent SAX. Results A two-compartment with additive model showed the pharmacokinetic process of SAX and 5-OH SAX, the concentration-effect relationship was represented by a sigmoidal E max model and sigmoidal E max with E 0 model for SAX and 5-OH SAX, respectively. Fitting parameters showed SAX was rapidly absorbed after administration ( T max =0.11 h, t 1/2, ka =0.07 h), widely distributed in the body (V ≈ 20 L/kg), plasma exposure reached 3282.06 ng*h/mL, and the elimination half-life was 6.13 h. The maximum plasma dipeptidyl peptidase IV (DPP-4) inhibition ratio of parent SAX was 71.47%. According to the final fitting parameter EC 50 , EC 50, 5−OH SAX =0.46EC 50, SAX(parent) , it was believed that the inhibitory effect of 5-OH SAX was about half of the parent SAX, which is consistent with the literature. Conclusions The PK-PD link model of the parent SAX established in this study can predict its pharmacokinetic process in T2DM rats and the strength of the inhibitory effect of DPP-4 based on non-clinical data.
研究领域:
药理学
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药代动力学
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药效学
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糖尿病研究
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分析化学
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DOI
PubMed
高影响因子
FOOD CHEMISTRY
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2026
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IF 10.4
Jialiang Zou,Huangsheng Zhang,Liang Zhao,Huanhuan Xu,Lin Chen,Hongping Chen,Fu Wang,Yuan Hu,Youping Liu
Chuan Chenpi (CCP), the peel of the ancient Chinese citrus variety Citrus reticulata ‘Dahongpao’, enhances its edible and medicinal value through aging. This study focuses on CCP samples aged 1–8 years, aiming to explore the dynamic changes during aging. Although aging induced noticeable changes in color, Fourier Transform Infrared (FTIR) analysis revealed no significant alterations in functional groups. Volatile and non-volatile metabolomic analyses indicated that aging primarily affects metabolite content rather than types, and both composition and antioxidant activity reached relatively high levels in the fourth year. The experimental results illustrate that the improvement in CCP quality induced by aging does not follow a linear pattern but exhibits fluctuations. The findings verify that the fourth year serves as a critical turning point for CCP's quality. This study clarifies the dynamic variation of chemical components in CCP during aging, thereby providing a scientific basis for the selection of its aging duration.
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高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
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2026
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IF 2.5
Huichao Wang,Yulong Ren,Rui Ao,XiuJuan Wang,Xiu-Li Xu,Jie Lian,Feng Zhang
A novel amine-functionalized magnetic covalent organic framework Fe 3 O 4 @COF-NH 2 , constructed from 1,3,5-tris( p -formylphenyl) benzene (TFPB) and 2,2′-dinitrobenzidine (2,2’-DNB), was rationally designed and synthesized for the first time. The resulting core-shell material, which features a facile synthesis, high stability, and tunable porosity, was employed as a highly efficient adsorbent for the magnetic solid-phase extraction (MSPE) of eleven mycotoxins from complex cereal matrices. Benefiting from its abundant active sites, the adsorbent exhibited excellent performance, driven by synergistic π-π stacking and hydrogen bonding interactions. Coupled with UPLC-MS/MS, the established method achieved a rapid and robust analysis with remarkably low limits of detection (0.02–0.10 μg/kg) and excellent recoveries (74.5%–99.5%). This work provides a powerful and practical platform for the high-throughput, sensitive, and reliable monitoring of multi-class mycotoxins, demonstrating significant advantages for food safety applications.
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高影响因子
CURRENT PHARMACEUTICAL BIOTECHNOLOGY
·
2026
·Vol. 27
·期 1
·76-94
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IF 2.6
Zhixin Wang,Shuqin Liu,Ying Zhang,Huaming Xian,Xinzhu Yuan,Changwei Lin,Xisheng Xie
Background Diabetic Kidney Disease (DKD) is a major cause of End-Stage Renal Disease (ESRD) and lacks effective treatments. Tangmaikang Granules (TMK), a multi-herb traditional Chinese medicine formulation, have shown potential in managing DKD. However, the precise active components, molecular mechanisms, and therapeutic advantages of TMK remain unclear. Objective This study tests the hypothesis that TMK granules exert protective effects on DKD by targeting multiple pathways involved in oxidative stress, inflammation, and apoptosis in podocytes through a multi-targeted approach. The aim was to identify TMK’s bioactive components, evaluate its therapeutic potential, and uncover its molecular mechanisms in DKD. Methods The bioactive constituents in TMK were determined through ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Drug targets were identified using SwissTargetPrediction and SuperPred, whereas DKD-associated targets were obtained from the GeneCards, DisGeNET, OMIM, and TTD databases. A Protein-Protein Interaction (PPI) network was constructed, and key targets were identified via topological analysis. Molecular docking and dynamics simulations were performed to evaluate stable binding interactions. GO and KEGG pathway enrichment analyses were conducted to uncover relevant signaling pathways. TMK's effects on oxidative stress, inflammation, and apoptosis in podocytes were assessed using CCK-8, flow cytometry, RT-qPCR, ELISA, and Western blot assays. Results Thirty active compounds and 384 potential therapeutic targets were identified, with eight key targets. Pathway enrichment analysis revealed TMK’s involvement in AGE-RAGE, EGFR, HIF-1, and apoptosis pathways, affecting inflammatory cytokine responses and oxidative stress. In vitro experiments demonstrated that TMK significantly reduced oxidative stress, inflammation, and apoptosis in podocytes by inhibiting the MAPK and NF-κB pathways. Conclusion TMK granules target DKD through a multi-component, multi-target strategy, effectively mitigating oxidative stress and suppressing inflammatory and apoptotic pathways. This study integrates advanced computational and experimental methods, demonstrating TMK’s unique therapeutic potential and providing a robust foundation for its clinical application in DKD management.
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高影响因子
JOURNAL OF HAZARDOUS MATERIALS
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2021
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IF 10.588
Likai Qi,Tian Dong,Xinyi Jiang,Jingjing Li,Bin Di,Fang Yan
Wastewater-based epidemiology (WBE) was a near-real-time monitoring strategy for illegal drugs. However, solid-phase extraction (SPE) widely used in WBE was time-consuming and labor-intensive to extract ultra-trace target compounds from wastewater. In this study, a convenient magnetic solid-phase extraction (MSPE) approach based on newly designed and synthesized polydopamine functionalized core-shell magnetic mesoporous silica (Fe 3 O 4 @nSiO 2 @mSiO 2 @PDA) nanocomposite was synthesized and firstly utilized for simultaneously extracting five amphetamine-type stimulants (ATSs) from wastewater samples. Subsequently, ultrahigh performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method coupled with optimal MSPE was developed for determination of ultra-trace ATSs in wastewater. The validation results indicated a favorable linearity ranging from 1 to 200 ng L −1 , low limit of detection (0.5–2.5 ng L −1 ), and qualified recovery (95.1–106.6%) and repeatability (0.6–6.2%). In addition, the Fe 3 O 4 @nSiO 2 @mSiO 2 @PDA nanoparticles could be reused for at least ten times without significant loss of the adsorption efficiencies of ATSs. Finally, the MSPE-UPLC-MS/MS method was successfully applied to real wastewater samples with the results that the preparation procedure was shrunk from 2 h to 30 min without obvious decline of extraction efficiency compared with the SPE. Hence, based on merits of the novel Fe 3 O 4 @nSiO 2 @mSiO 2 @PDA nanocomposite, the proposed method is convenient and reliable for determination of ATSs in wastewater.
研究领域:
分析化学
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环境科学
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法医学
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DOI
PubMed
高影响因子
TALANTA
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2020
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IF 5.339
Yiyuan Zhou,Jiabi Xu,Nan Lu,Xinyu Wu,Yu Zhang,Xiaohong Hou
MIL-101(Cr) and graphene aerogel (GA) were hybridized as a multifunctional adsorbent for the preconcentration of trace analytes. The novel MIL-101(Cr)@GA was prepared and characterized by FTIR, XRD and SEM, where GA is serving as a carrier for MIL-101(Cr). The synthesized composite as a solid phase extraction (SPE) sorbent combined with UPLC-MS/MS was applied for the determination and quantification of five NSAIDs (phenacetin, meloxicam , naproxen , diclofenac sodium and carprofen) in different environmental water samples. The parameters influencing the whole extraction process were systematically optimized. Under the most favorable. conditions, good sensitivity was achieved with a limit of detection between 0.006 and 0.012 ng mL −1 , the linear range of 0.02–2 ng mL −1 for phenacetin , meloxicam and 0.05–5 ng mL −1 for naproxen , diclofenac sodium , carprofen ( r 2 ≥ 0.9940). The satisfactory recoveries of the target analytes were in the range from 77.2 to 103.3% with relative standard deviation (RSD) from 0.6% to 8.4%. The established method was proved to be simple, highly sensitive and accurate. The adsorbent could be reusable up to nine cycles without any decrease in performance, which provides economic strategy and little waste generation. Adsorption behaviors were explored by choosing two typical types of NSAIDs as models to measure the adsorption capacity of MIL-101(Cr)@GA. The maximum adsorption capacities for PHE and NAP were 232.5 and 333.3 mg g −1 , respectively.
研究领域:
环境科学
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分析化学
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DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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2023
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IF 3.4
Pan Hu,Xin Yan,Yijia Zeng,Zherui Jiang,Juan Liu,Wu-wen Feng
Botanic polysaccharides can be metabolized by gut microbiota into short-chain fatty acids (SCFAs) to exert extensive bioactivities, yet targeted analysis of the effect of botanic polysaccharides on other gut microbial metabolites is scarcely seen. Tryptophan metabolites such as indole and indole derivatives play import roles in health and disease development. Using polysaccharides from Atractylodes macrocephala Koidz. (AMP) in treating ulcerative colitis as the example, we checked the effects of AMP on tryptophan metabolites. After examination of pharmacological effects of AMP, we established an ultra-performance liquid chromatography coupled with mass spectrometry/mass spectrometry (UPLC-MS/MS) method to simultaneously determinate the levels of 30 tryptophan metabolites and used the method to determine the levels of these metabolites in feces and plasma. The detection results showed that 12 metabolites in feces can be detected, and 17 metabolites can be detected in plasma samples. In addition, we found out that total levels of aryl hydrocarbon receptor ligands were decreased in colitis model whereas AMP treatment can increase the levels of total ligands in both feces and plasma. The results indicated that the therapeutical effect of AMP on colitis was associated with modulation of fecal and host tryptophan metabolism. This study provides new insight into the molecular mechanisms of polysaccharides that the beneficial effects of polysaccharides can be achieved by modulating microbial tryptophan metabolism in addition to SCFAs.
研究领域:
药理学
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微生物学
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分析化学
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PubMed
高影响因子
危险品化学品经营许可证（带存储）