FOOD CHEMISTRY
·
2025
·
IF 9.8
You Long,Yuting Wang,Gan Zhang,Bei Gan,Qiang Yu,Jianhua Xie,Xinyi Zang,Yi Chen
Enniatin and Alternaria mycotoxins have presented adverse effects to food safety and human health, and an accurate, simultaneous analytical method for these mycotoxins was promising. This study reported the synthesis of a magnetic covalent organic framework (NH 2 -Fe 3 O 4 @TpBD-COF) for efficient extraction of seven mycotoxins from wheat, coupled to UPLC-MS/MS for simultaneous quantification. The magnetic solid phase extraction (MSPE) parameters, including adsorbent dose (10 mg), vortex duration (5 min), and extraction/elution solvents (ACN/MeOH, 6/4, v /v), were systematically optimized. Method validation revealed ultra-low limits of quantification (LOQs:0.03 to 0.5 μg kg −1 ), matrix effects (ME<8.49 %), recovery rates(81.3 %–109 %), and precision (RSD < 9.70). The adsorbent maintained satisfactory performance through 8 reuse cycles. Density functional theory (DFT) calculation indicated exergonic adsorption, primarily driven by hydrogen bonding, van der Waals forces, and hydrophobic interactions. The integrated method offers a sensitive and accurate approach for emerging mycotoxin analysis in wheat, potentially mitigating associated health risks.
研究领域:
食品安全
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分析化学
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真菌毒素学
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材料科学
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环境卫生
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DOI
PubMed
高影响因子
CURRENT DRUG METABOLISM
·
2021
·Vol. 22
·期 1
·70-82
·
IF 3.731
Zuo Lihua,Li Jia,Xue Lianping,Jia Qingquan,Li Zhuolun,Zhang Mengya,Zhao Mengfan,Wang Mengli,Kang Jian,Du Shuzhang,Sun Zhi
Background: Alpiniae oxyphyllae Fructus (AOF), a traditional Chinese medicine (TCM), is widely used in the treatment of urinary, gastrointestinal and neurologic diseases in China. Although terpenoids are the main active ingredients of AOF, there are few researches on their pharmacokinetics
and metabolism. Methods: In this study, a sensitive, rapid, accurate and novel ultra high performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) method was established to evaluate the pharmacokinetic behavior of five terpenoids (oxyphyllenodiol B, (4S* ,5E,10R*)-7-oxo-tri-nor-eudesm-5-en-4β-ol,
7-epi-teucrenone, (+)- (4R,5S,7R)-13-hydroxynootkatone, (E)-labda-12,14-dien-15(16)-olide-17-oic acid) in rats after oral administration of AOF extracts. 27 metabolic metabolites of the five terpenoids were identified by ultra high performance liquid chromatography -Q Exactive hybrid quadrupole-orbitrap
high-resolution accurate mass spectrometry (UHPLC-Q-Orbitrap HRMS) based on precise mass and fragment ions. Results: The established pharmacokinetic analysis method showed good linearity over a wide concentration range, and the lower quantitative limit (LLOQ) ranged from 0.97 to 4.25
ng/mL. Other validation parameters were within the acceptable range. In addition, 27 metabolites were identified in plasma, urine and feces samples, and the metabolic pathways of five terpenoids were mainly focused on glucoside conjugation, dehydration, desaturation and glycine conjugation.
Conclusion: This is the first study on the pharmacokinetics and metabolism of five terpenoids in AOF, illuminating the disposal process of terpenoids in vivo. It was expected that the results of this study would provide some references for the apprehension of the action mechanism and
the further pharmacological study of five terpenoids in AOF.
研究领域:
中药学
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分析化学
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药理学
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高影响因子
RSC Advances
·
2026
·Vol. 16
·期 31
·28230-28242
·
IF 6.1
Jin-tuo Yin,De-mao Wang,Xue-chun Wu,Juan Lu,Zheng-ming Qian,De-qiang Li,Rui Feng
Taihangia rupestris Yu & Li (T. rupestris) was a nationally protected plant and its active compounds exhibit antidiabetic potential, but systematic phytochemical and pharmacological investigations remain limited. To balance conservation and utilization, the chemical composition and bioactivities (antioxidant and α-glucosidase inhibitory effects) of wild and cultivated T. rupestris were compared, followed by active compound screening. UPLC-MS/MS was used to identify chemical constituents in wild, mountain-cultivated, and foothill-cultivated samples, with multivariate analysis for differential components. The TFC and TPC, and the antioxidant capacity were evaluated via FRAP, CUPRAC, TRC, and DPPH assays. Additionally, α-glucosidase inhibition was assessed via IC50 determination. Online HPLC-ABTS and ultrafiltration-LC/MS (UF-LC/MS) were employed to screen antioxidants and α-glucosidase inhibitors (α-GIs), respectively, with molecular docking validating binding mechanisms. As a result, among 114 identified compounds, 111 showed significant environment-dependent variations, primarily flavonoids, phenolics, and terpenoids. Foothill-cultivated plants exhibited upregulated flavonoids/phenolics (e.g., rutin and gallic acid derivatives, P < 0.05) and superior antioxidant activity (Trolox equivalents: FRAP 367.18 ± 1.03; CUPRAC 572.40 ± 0.82) and α-glucosidase inhibition (IC50 0.2775 µg mL−1) versus wild (IC50 0.4948 µg mL−1) and mountain-cultivated samples (IC50 0.5425 µg mL−1). Ten antioxidants were screened, with seven also acting as α-GIs. UF-LC/MS and docking confirmed 8 α-GIs (binding energy < −5 kcal mol−1), where phenolic hydroxyl groups formed hydrogen bonds with ASP residues of α-glucosidase. Cultivated T. rupestris (especially foothill-grown) outperformed wild plants in bioactives composition and efficacy, serving as a sustainable alternative. Flavonoids and phenolics contributed to its antidiabetic potential via dual antioxidant and enzyme-inhibitory effects, supporting further pharmaceutical development.
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高影响因子
ULTRASONICS SONOCHEMISTRY
·
2026
·
IF 10.2
Yaru Ji,Xinyue Liu,Mengyang Hou,Shuai Hao,Yangyang Ye,Yu Rao
Large quantities of agri-food by-products arise from citrus processing, creating disposal challenges but also opportunities for valorization. To address this, this study aimed to recover bioactive phenolics from C itrus aurantium leaves (CAL) and to define their composition and bioactivity. First, was screened 16 ionic liquids and identified 1-hexyl-3-methylimidazolium chloride ([C 6 mim]Cl) as the optimal-polarity solvent for phenolic extraction. Building on this, an ionic liquid–ultrasound synergistic extraction (IL–USE) process was developed and optimized using single-factor experiments combined with response surface methodology. Under the optimal conditions (0.35 mol/L [C 6 mim]Cl, liquid-to-solid ratio 27 mL/g, ultrasonic power 280 W, 50 min, 55 °C), the total phenolics yield reached 80.57 ± 0.60 mg/g. Compared with ultrasound-assisted extraction and conventional heat-reflux extraction, IL-USE delivered higher yields. This enhancement was macroscopically reflected in the scanning electron microscopy (SEM) analysis, which revealed more pronounced cell-wall disruption. For downstream enrichment, among five macroporous resins evaluated, HPD-826 performed best, and subsequent optimization of breakthrough and elution parameters afforded a CAL total phenolics (CAL-TP) fraction with 77.45 ± 1.63% purity. Furthermore, UPLC-QTOF-MS/MS tentatively identified 47 constituents, establishing a robust chemical profile of CAL-TP. Functionally, in insulin-resistant HepG2 cells, CAL-TP increased glucose consumption and glycogen synthesis and enhanced hexokinase and pyruvate kinase activities, thereby indicating hypoglycemic potential. Collectively, this study provides a green and efficient process that yields phenolic-rich fractions from CAL with defined composition and promising antidiabetic activity.
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PubMed
高影响因子
CHEMICO-BIOLOGICAL INTERACTIONS
·
2026
·
IF 5.2
Peiqi Wang,Yan Chen,Jun Wu,Shiqi Jiang,Lu Cao,Ren-ai Xu,Xiaoqun Xu
Bosutinib is a second-generation tyrosine kinase inhibitor (TKI) primarily used for the treatment of chronic myeloid leukemia (CML). The aim of this study was to develop and validate a rapid and accurate ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) method for the simultaneous determination of bosutinib and its major metabolite M5. Chromatographic separation was performed on an Acquity UPLC BEH C18 column (2.1 mm × 50 mm, 1.7 μm) using a gradient elution with acetonitrile and 0.1% formic acid as the mobile phase, and gefitinib was used as the internal standard (IS). Biological analysis showed that both bosutinib (2-400 ng/mL) and its metabolite M5 (1-60 ng/mL) exhibited good linearity in their respective concentration ranges, with correlation coefficients ( r 2 ) of 0.996 and 0.993, respectively. Both of them exhibited intra- and inter-day precision (RSD%) below 15% and accuracy (RE%) within ± 15%. Recoveries were all within the range of 85.3-98.0%, and matrix effects were all within the range of 91.6-101.6%. Ultimately, human liver microsomes (HLM) was used to study in vitro metabolic stability, while in vivo pharmacokinetics were evaluated in rats. In vivo pharmacokinetic studies confirmed that this method could be successfully used for the analysis of bosutinib after oral administration of 50 mg/kg in rats. In vitro results showed that bosutinib had the intrinsic clearance (CL int ) value of 0.03 mL/min/mg and the half-life (t 1/2 ) value of 79.94 min. This study provides a potential reference for the clinical investigation of bosutinib.
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高影响因子
FOOD RESEARCH INTERNATIONAL
·
2025
·
IF 8
Hui Zhang,Mengjia Xu,Ming Yang,Jun Ding,Mingquan Guo
The seeds of Cassia obtusifolia L. (Cassia seed) have long been utilized as an edible traditional Chinese medicinal herb and tea with various health benefits, including improving obesity and protecting eyesight. In this work, we developed a rapid screening method based on pancreatic lipase (PL)-functionalized magnetic composite nanoparticles coupled with ultra-performance liquid chromatography-quadrupole-time of flight mass spectrometry (UPLC-QTOF-MS/MS) and molecular networking analysis. This method utilized the advantages of polydopamine (PDA) and metal-organic frameworks (MOFs) functionalized magnetic core-shell structures (Fe 3 O 4 @PDA@MOFs MNPs), significantly enhancing the immobilization efficiency and performance of PL. The enzyme loading capacity was increased by 1.5-fold, and notable improvements in reusability and storage stability were also observed. By using this immobilized enzyme model in combination with UPLC-QTOF-MS/MS, 22 potential PL inhibitors were selectively screened and identified from the seeds of Cassia obtusifolia L. Molecular network analysis was innovatively introduced to improve the efficiency of compound identification by summarizing the similarity of mass spectral fragments. The inhibitory activities of three representative ligands of Cassiaside B, Biochanin A 7-glucoside and Aurantio-obtusin were further investigated. Molecular docking analysis revealed that the amino acid residue ASP249 in lipase contributes a significant role in the binding of active ligands to lipase. Overall, this proposed screening strategy, characterized by its specificity in enzyme binding and the convenience of functionalized magnetic separation, presents promising prospects for rapid and high-throughput screening of active components and drug candidates from natural resources.
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高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2025
·
IF 2.8
Cuiyao He,Saisai Ling,Ying Jin,Lisha Fu,Xiaoke Dai,Xiaohui Qi,Yiying Wu,Zhenglei Wang,Yuhua Deng
Piperacillin/tazobactam and metronidazole are two commonly antimicrobials used to prevent and treat infections after liver transplantation in pediatric patients. However, under the recommended dose, it may lead to insufficient antimicrobial treatment and poor efficacy. To achieve antimicrobial therapy based on pharmacokinetic strategies, a rapid and highly sensitive ultra-high performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) method was developed to measure the plasma concentrations of piperacillin, tazobactam, and metronidazole in pediatric liver transplant recipients. Sample separation was achieved using an Acquity UPLC CSH C 18 column (2.1 × 50 mm, 1.7 μm) with gradient elution. The mobile phase consisted of ammonia solution–formic acid–water (0.5:1:1000, v / v /v) and methanol–acetonitrile (1:1, v/v). The plasma concentration range was 0.20–100.00 μg/mL, with good linear range. The intra- and inter-day precisions were less than 13.4 %, and the accuracy ranged from 90.0 % to 109.0 %. The selectivity, carryover, dilution integrity, matrix effect, recovery, and stability met the requirements of the relevant guidelines. The established UPLC–MS/MS method was successfully applied to measure the concentrations of piperacillin, tazobactam, and metronidazole in the plasma of pediatric liver transplant patients. The results showed that according to the recommended dosing regimen, piperacillin/tazobactam reached the effective therapeutic target of 50 %T > MIC in only 4 h. The maximum plasma concentration (C max ) of metronidazole ranged from 9.46 to 28 μg/mL, with an average C max of 16.59 μg/mL, which did not achieve the ideal C max /MIC ratio of 8–10.
研究领域:
临床医学
·
药理学
·
移植学
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PubMed
高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2025
·Vol. 39
·期 5
·e70055
·
IF 1.7
Nan Guo,Sheng Hu,Yahui Zhang,Wen Zhang,Dejun Li,Yue Tang,Zijian Tai,Xin Guo,Bing Leng
Tigecycline has been widely used for treating infections caused by multidrug resistant bacteria, but the dosage and intrapulmonary distribution were still controversial. In this study, a UPLC–MS/MS method was established and fully validated to quantify tigecycline in human plasma and BALF. A simple and rapid protein precipitation was used to extract the analytes from plasma and BALF samples. Then, tigecycline and IS were separated on a SHIMADZU AQ-C18 column and detected using electrospray ionization positive ion mode using the transitions of m / z 586.3 → 513.2 m / z for TGC and 458.0 → 441.0 m / z for minocycline (IS). The linearity of the calibration was in the range of 20–2000 ng/mL in plasma and BALF. The validated method was successfully applied to investigate pharmacokinetic characteristics of tigecycline in critically ill patients. The results suggested that after intravenous administration of 100-mg q12h tigecycline, the AUC 0–12 was 3663.02 ± 2075.84 ng × h/mL and C ss,av was 305.25 ± 172.99 ng/mL; the average plasma concentration/ELF concentration ratio was 3.66. Significant individual differences and highly variable pharmacokinetic properties were observed, indicating that adjustment of dosing regimens according to therapeutic drug monitoring is effective and efficient to guarantee the drug efficacy and safety especially for critically ill patients.
研究领域:
临床医学
·
药理学
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DOI
PubMed
高影响因子
ULTRASONICS SONOCHEMISTRY
·
2025
·
IF 9.7
Ziyu Lv,Jing Ma,Chi Wei,Jiaqi Wang,Dan Wang,Xinxin Cheng,Guoliang Chen,Luis A.J. Mur,Yanfeng Wang,Duo Cao
Bitter orange flowers (BOF), a renowned medicinal and edible botanical resource, are rich in phenolic compounds with significant potential for health and industrial applications. However, efficient extraction and purification techniques for recovering bioactive phenolics remain underexplored. To address this gap, this study aimed to develop an eco-friendly integrated strategy combining natural deep eutectic solvent-ultrasound synergistic extraction (NADES-USE) with adsorptive purification for efficient recovery of total phenolics from BOF (BOF-TP). First, choline chloride-ethylene glycol (ChCl-EG) was determined to be the optimal extraction solvent from 12 synthesized NADESs and 3 common solvents. Employing Box-Behnken design (BBD), the optimized parameters for NADES-USE (38 % aqueous ChCl-EG, 18 mL/g, 345 W, 43 min, and 55 °C) resulted in a BOF-TP yield of 104.58 ± 0.34 mg/g, which was 1.30 to 2.16 times higher than those achieved with conventional solvents. Then, AB-8 resin demonstrated optimal adsorption–desorption performance for BOF-TP, with adsorption behavior strongly conforming to Langmuir isotherm and pseudo-second-order kinetic models. Thermodynamic analysis confirmed a spontaneous, exothermic physisorption process with decreasing entropy. The breakthrough curves and gradient elution curves were utilized to establish a chromatographic purification process for crude BOF-TP extracts, achieving a purity of 75.62 ± 0.95 %. Finally, a validated UPLC-Q/TOF-MS/MS method facilitated comprehensive chemical characterization and simultaneous quantification of seven bioactive compounds, serving as a basis for the quality control of purified BOF-TP extracts. In conclusion, this work demonstrates that the combination of NADES-USE and adsorptive purification offers significant potential for producing highly purified BOF-TP extract for further use in food and pharmaceutical applications.
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高影响因子
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2025
·
IF 3.8
Xie Baogang,Zhan Dujuan,Wu Le,Wang Lele,Lei Yongrong,Liu Meng,Liu Xiaodan,Li Suping
Congenital heart disease (CHD) poses significant clinical challenges due to limitations in early prenatal diagnosis. This study aimed to identify serum metabolic biomarkers for CHD using a combined metabolomics approach. Serum samples from 55 pregnant women carrying fetuses with confirmed CHD (CHDP group) and 49 healthy controls (ZCP group) were analyzed via non-targeted 1 HNMR metabolomics, revealing distinct metabolic profiles. Six choline pathway metabolites were further quantified by ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Among these, N,N-dimethylglycine (DMG) exhibited the most significant reduction in the CHDP group (1.07 ± 0.03 vs. 1.55 ± 0.04 µg/mL, p < 0.001), with an area under the ROC curve (AUROC) of 0.883 in the discovery cohort. Validation in an independent cohort (58 CHDP vs. 62 ZCP) confirmed DMG’s diagnostic potential (AUROC = 0.818). While betaine-homocysteine methyltransferase 2 (BHMT2) activity showed no intergroup differences, DMG’s consistent performance highlights its utility as a non-invasive biomarker. This study underscores the clinical value of metabonomics in prenatal CHD screening and establishes DMG as a promising diagnostic marker, potentially improving early detection and perinatal management. Graphical abstract
研究领域:
代谢组学
·
儿科心脏病学
·
产前诊断
·
生物医学研究
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PubMed
高影响因子
MICROCHEMICAL JOURNAL
·
2026
·
IF 5.2
Long Xu,Xiang Liang,Mengqing Xiao,Walter Vetter,Shuaishuai Yang,Kai Chen,Fashan Wei,Xiaoling Yu,Xia Shen,Mingjiang Zhu
A 3-tier screening strategy-based LC-MS/MS profiles FAHFAs in fruit seeds and pits. • Fruit seed oils contain significantly higher total FAHFA levels than pit oils. • Bayberry seed oil is the richest FAHFA source (168 ng/g) among all samples. • OAHOA and PAHOA are identified as predominant FAHFA species in fruit seeds. Fatty acid esters of hydroxy fatty acids (FAHFAs) are bioactive lipids with anti-inflammatory and antidiabetic properties, but their occurrence in fruit seeds and pits remain largely unexplored. Here, untargeted lipidomics and fatty acid profiling were firstly employed to characterize the overall lipid landscape and precursor pools. Subsequently, a targeted platform was established by integrating solid-phase extraction (SPE) enrichment, N , N -dimethylethylenediamine (DMED) derivatization, and UPLC-ESI-MS/MS in multiple reaction monitoring (MRM) mode. Using a predictive MRM database covering 2116 theoretical FAHFA species and a three-tier screening strategy (two MRM filtering rounds followed by retention time and signal-to-noise evaluation), 49 endogenous species were identified in 17 fruit seeds and 4 fruit pits. It was found that fruit seed oils contained significantly higher total FAHFA levels than pit oils (3–168 vs. 1–35 ng/g), with bayberry seed oil showing the highest content (168 ng/g). Predominant species included OAHOA, LAHLA, PAHOA, and OAHSA. This first comprehensive FAHFA profile, achieved via the three-tier strategy, establishes seed oils as notable dietary sources of these lipids and offers a robust platform for discovering bioactive lipids in complex plant matrices. Download: Download high-res image (113KB) Download: Download full-size image
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高影响因子
FOOD RESEARCH INTERNATIONAL
·
2023
·
IF 8.1
Ziwei Wang,Lin Zhou,Wenqian Hao,Yu Liu,Xia Xiao,Xiao Shan,Chenning Zhang,Binbin Wei
P. pseudocerasus and P. tomentosa are the two native Chinese cherry species of high economic and ornamental worths. Little is known about the metabolic information of P. pseudocerasus and P. tomentosa . Effective means are lacking for distinguishing these two similar species. In this study, the differences in total phenolic content (TPC), total flavonoid content (TFC), and in vitro antioxidant activities in 21 batches of two species of cherries were compared. A comparative UPLC-QTOF/MS-based metabolomics coupled with three machine learning algorithms was established for differentiating the cherry species. The results demonstrated that P. tomentosa had higher TPC and TFC with average content differences of 12.07 times and 39.30 times, respectively, and depicted better antioxidant activity. Total of 104 differential compounds were identified by UPLC-QTOF/MS metabolomics. The major differential compounds were flavonoids, organooxygen compounds, and cinnamic acids and derivatives. Correlation analysis revealed differences in flavonoids content such as procyanidin B1 or isomer and (Epi)catechin. They could be responsible for differences in antioxidant activities between the two species. Among three machine learning algorithms, the prediction accuracy of support vector machine (SVM) was 85.7%, and those of random forest (RF) and back propagation neural network (BPNN) were 100%. BPNN exhibited better classification performance and higher prediction rate for all testing set samples than those of RF. The study herein found that P. tomentosa had higher nutritional value and biological functions, and thus considered for usage in health products. Machine models based on untargeted metabolomics can be effective tools for distinguishing these two species.
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高影响因子
危险品化学品经营许可证（带存储）