ANALYTICAL BIOCHEMISTRY
·
2023
·
IF 2.9
Yao Liu,Zhichao He,Heng Liang,Minzhen Han,Jinxingyi Wang,Qian Liu,Yanping Guan
Rapidly developing UHPLC-MS/MS bioassays with high throughput and quality are challenging yet desired in routine clinics. Methods & results A high-throughput UHPLC-MS/MS bioassay has been built for simultaneously quantifying gefitinib , ruxolitinib , dasatinib , imatinib , ibrutinib , methotrexate , cyclophosphamide and paclitaxel . After the protein precipitation with methanol, samples were separated on an Acquity BEH C 18 column following a gradient elution system with methanol and 2 mM ammonium acetate in water at 40 °C with a run time of 3 min (flow rate 0.4 mL/min). Mass quantification in the positive ion SRM mode was then performed with electrospray ionization . The method of specificity, linearity, accuracy, precision, matrix effects, recovery, stability, dilution integrity and carryover were all validated as per the guideline of the China Food and Drug Administration whose values met the admissible limits. Application of the bioassay to therapeutic drug monitoring revealed important variability in the studied anti-tumour drugs. Conclusion This validated approach was shown to be reliable and effective in clinical management, being a valuable support in therapeutic drug monitoring and subsequent individualized dosing optimization.
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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DOI
PubMed
高影响因子
Bioanalysis
·
2023
·
IF 1.8
Liyuan Cheng,Xiaoying Zhang,Jige Qi,Yue Zhang,Kun Zhou
Aim: To develop a UHPLC–MS/MS method for the quantification of 12 constituents in rat plasma after oral administration of Zhuanggu Guanjie. Methods: Constituent separation was performed on a C18 column, and the mass spectrometric detection was performed in multiple reaction monitoring mode with a positive–negative ionization mode. Results: The method was successfully applied to the pharmacokinetic study of these 12 constituents after rats taking Zhuanggu Guanjie capsules. The results showed that psoralen, isopsoralen and aspersaponin VI were the key effective components and had high exposure. Conclusion: A rapid, simple and sensitive ultra-high-performance liquid chromatography coupled with triple quadrupole mass spectrometry method for the detection of 12 components in rat plasma after taking Zhuanggu Guanjie was developed and applied in this pharmacokinetics study.
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高影响因子
PHYTOMEDICINE
·
2025
·
IF 8.3
Meng Zhang,Rui Liu,Ting Zhou,Yuxin Guo,Hui Li,Wei Wu
Background Chronic fatigue syndrome (CFS) is a crippling illness with limited effective treatment options. Recent findings have suggested that ginseng stem and leaf saponins (GSLS) possess anti-fatigue effects. However, the detailed mechanisms by which GSLS impact CFS have yet to be fully elucidated. Purpose This study aimed to explore the efficacy and underlying mechanisms of GSLS in the treatment of peripheral and central fatigue in mice with CFS. Methods A CFS model was established in male C57BL/6 mice, which were then subjected to prolonged swimming tests. The validity of this model and the efficacy of GSLS were verified using the forced exhaustion swimming test and the Morris water maze test. The anti-fatigue mechanism of GSLS was verified using pathological section observations, biochemical index tests, neurotransmitter analysis, and Ultra-high performance liquid chromatography–high-resolution mass spectrometry (UHPLC-MS) metabolomics analysis. Results GSLS prolonged the swim time-to-exhaustion in CFS mice and reduced escape latency in the water maze, revealing their anti-fatigue and memory-improving effects. GSLS significantly protected both peripheral (liver) and central (hippocampus) tissues, as shown in pathological sections. Biochemical indices suggested that GSLS mitigate peripheral fatigue by reducing energy expenditure and oxidative damage and inhibiting the production of harmful metabolites. Furthermore, GSLS altered the abnormal levels of 14 neurotransmitters in the brains of CFS mice, including seven upregulated and seven downregulated neurotransmitters, highlighting their role in mitigating central fatigue through neurotransmitter regulation. Serum metabolomics analysis identified alterations in 19 metabolites across 11 metabolic pathways, thereby elucidating the potential mechanisms by which GSLS treat CFS. Conclusion GSLS ameliorate damage caused by both peripheral and central fatigue. They also act on multiple pathogenic mechanisms by modulating neurotransmitters and serum biomarkers, making them a potential therapeutic agent for CFS.
研究领域:
药理学
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代谢组学
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神经科学
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DOI
PubMed
高影响因子
PHYTOCHEMICAL ANALYSIS
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2026
·
IF 2.9
Mengyuan Wu,Zhaojie Ji,Yanjiang Dong,Sitong Liu,Shuo Diao,Xintong Wang,Ju Zhao,Boya Zhang,Da Rong,Wenxin Xu,Enli Wang,Rui Niu,He Xiao,Mingming Yu,Zhihua Lv,Sherwin K. B. Sy,Hai Yang
Objectives This study aimed to develop and validate a UHPLC-MS/MS method for the simultaneous determination of 14 constituents related to Renshen Guben Oral Liquid (RSGB) in human plasma and to explore concentration–absolute neutrophil count (ANC) associations in cancer patients with chemoradiotherapy-induced neutropenia (CIN). Methods Candidate constituents were selected by integrating chemical representativeness, disease relevance, reference standard availability, and analytical feasibility, with support from network pharmacology. Plasma samples were collected from 25 patients before administration and at 1 and 2 h after RSGB administration. Samples were processed by liquid–liquid extraction using methyl tert-butyl ether or n-butanol and analyzed by UHPLC-MS/MS. Spearman correlation analysis was used to assess exploratory associations between post-dose concentrations of major quantifiable circulating constituents and ANC change from baseline to Day 15. Results The assay fulfilled predefined bioanalytical acceptance criteria and enabled simultaneous quantification of 14 RSGB-related constituents in human plasma. Ginsenoside Rb1 (G-Rb1), ginsenoside compound K (G-CK), and paeonol (PAE) were the major quantifiable circulating constituents, whereas protopanaxadiol (PPD) and protopanaxatriol (PPT) were only sporadically quantifiable. Exploratory analyses showed positive associations between concentrations of G-Rb1, G-CK, and PAE and ΔANC. Molecular docking provided complementary computational support for potential target interactions. Conclusions G-Rb1, G-CK, and PAE were the major quantifiable circulating RSGB-related constituents within the early sampling window, and their concentrations showed exploratory associations with ANC change. These findings provide complementary in vivo evidence for evaluating RSGB-related constituents.
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DOI
高影响因子
Journal of Pharmaceutical Analysis
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2026
·
IF 11.2
Jialong Jing,Ning Sheng,Zhe Wang,Jinlan Zhang
α,β-Unsaturated aldehydes (enals) are primarily metabolized via glutathione (GSH) conjugation, forming GSH–enal adducts, which represent the major pathway for their in vivo clearance and detoxification. These adducts undergo further metabolism to form GlyCys–enal adducts, Cys–enal adducts, and N-acetylcysteine (NAC)–enal adducts, ultimately excreted in urine. Elucidating the mechanisms by which enals undergo detoxification through GSH conjugation, metabolism, and excretion is important for understanding their roles in related diseases. However, comprehensive characterization of enal adducts remains challenging because of their structural instability and low concentrations in vivo . In this study, a novel strategy was developed to characterize the in vivo metabolism of GSH–enal adducts using liquid chromatography-mass spectrometry (LC-MS) combined with 2,4-dinitrophenylhydrazine derivatization. Characteristic fragment ions and fragmentation patterns were summarized based on 56 synthetic enal adducts analyzed by high-resolution MS. Based on the GSH–enal metabolic pathway, a database containing 4,496 predicted enal adducts was constructed to facilitate the discovery and identification of potential enal adducts. Using precursor ion scanning by LC-MS/MS integrated with the predicted database and characteristic fragment ions, 499 candidate enal adducts were initially detected in rat heart, liver, and kidney tissues. Among these, 49 novel enal adducts were further identified using dynamic multiple reaction monitoring, and 12 of the identified enal adducts were confirmed using synthetic standards. This strategy was successfully applied to dynamically profile GSH–enal adducts and their metabolites in rats with myocardial ischemia (MI), representing the first comprehensive elucidation of the detoxification and metabolic pathways of oxidative stress-induced enals. These findings provide new insights into the dynamic changes of enals and GSH–enal adducts during disease-associated oxidative damage.
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DOI
高影响因子
MICROCHEMICAL JOURNAL
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2026
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IF 5.1
Ruifeng Lin,Huiqiang Feng,Zhixin Zhang,Yanling Liu,Hongting Wen,Hulan Chen,Yu Fan,Yuzhu Tan,Zhentao Tang
To overcome the great challenge of simultaneously reducing the matrix effect and sensitively analyzing multi-mycotoxins in complex samples, a modified QuEChERS-UHPLC-MS/MS method based on novel nanomaterials was developed for the analysis of 18 mycotoxins in different matrices. The modified QuEChERS integrated traditional QuEChERS with freezing and magnetic dispersion solid phase extraction (MDSPE), which adopted an in-house fabricated nanomaterial (Fe 3 O 4 @MWCNT@Uio-67) as a purification material. To validate the sensitive and efficient analysis of the target mycotoxins, the established method was investigated on three medicinal and edible matrices. These matrices are typical representatives of complex and diverse matrices, of which the main ingredients are starch, oil, and polysaccharides, respectively. Under the optimized conditions, the linear detection range was 1.00–1250.00 μg/kg (R 2 > 0.998). The detection limits were down to 0.003–5.096 μg/kg. The accuracy (spiked recovery/66.38–139.17%) and precision (intra-RSDs/0.15–19.65%, inter-RSDs/0.23–16.40%) were both satisfactory. Compared to C 18 , the novel material presented a better ability to purify the substrate matrices, along with a more acceptable recovery. Through the comparison with other methods, the developed method was further demonstrated to be sensitive, efficient, and with great potential for the analysis of multi-mycotoxins in diverse and complex samples.
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高影响因子
Food & Function
·
2021
·Vol. 12
·期 24
·12683-12695
·
IF 5.396
Zhou Lu,Yat-Tin Chan,Kenneth Ka-Hei Lo,Vincy Wing-Si Wong,Yuk-Fan Ng,Shi-Ying Li,Wing-Wa Ho,Man-Sau Wong,Danyue Zhao
Dietary polyphenols are phytonutrients exhibiting multiple health benefits in humans including those in infants. However, data on breast milk (poly)phenolic composition are limited, especially among Asian populations. This study aimed to assess the levels of dietary polyphenols and their microbial-derived metabolites in the breast milk of Hong Kong lactating women, and how maternal diet correlated with the phenolic composition in breast milk. Breast milk samples from 89 healthy Hong Kong lactating women (aged 19–40 years) were collected. Maternal intake of plant-based foods and polyphenols was estimated through 3-day dietary records and the Phenol-Explorer database. Twelve commonly consumed polyphenols including their microbial-derived metabolites in breast milk were quantified using an optimized and validated UHPLC-MS/MS method. The effect of maternal intake on breast milk phenolic levels was then examined via the Pearson correlation test. The mean concentrations of individual phenolic compounds ranged from 5.1 nmol L−1 (chlorogenic acid) to 731.5 nmol L−1 (3,4-dihydroxybenzoic acid). Despite suboptimal intake of fruits and vegetables among our participants, breast milk phenolic levels were comparable to those of foreign populations. Significant correlations were found between dietary intake and multiple phenolics, particularly legume and daidzein (r = 0.33, P = 0.001), and tea and epicatechin (r = 0.30, P = 0.03). Regarding phenolic metabolites, 3,4-dihydroxyphenylacetic acid was significantly correlated with several polyphenols, particularly quercetin (r = 0.34, P = 0.002), and equol was exclusively correlated with daidzein (r = 0.46, P < 0.001). Our findings support that intake of plant-based foods significantly affects breast milk phenolic composition. Future investigation on the bioavailability and health outcomes in infants is warranted to substantiate the transferability of these bioactive phytonutrients from mother to child through lactation, and to promote maternal intake of polyphenol-rich foods.
研究领域:
营养学
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饮食科学
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分析化学
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母婴健康
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植物化学
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF MASS SPECTROMETRY
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2026
·Vol. 61
·期 8
·e70082
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IF 2.1
Jiarui Zhang,Sijia Tong,Hongjie Ju,Hui Miao,Yujuan Gong,Meiyun Shi,Lei Yin
Neonicotinoid insecticides, such as imidacloprid, pose significant risks to aquatic ecosystems due to their widespread use and potential for accumulation. In this study, a sensitive and robust analytical strategy based on ultra-high performance liquid chromatography–tandem mass spectrometry (UHPLC–MS 3 ) was developed and validated for the determination of imidacloprid in multiple complex zebrafish biological matrices, including the muscle, liver, intestine, heart, brain, and gills. By harnessing the unique selectivity of the MS 3 acquisition mode, the method effectively eliminated endogenous matrix interferences and achieved a 243-fold enhancement in signal intensity compared to the conventional multiple reaction monitoring (MRM) mode. The sample pretreatment utilized a streamlined protein precipitation approach with methanol, ensuring high extraction efficiency and reproducibility across all tissues. The method was fully validated according to FDA guidelines, demonstrating excellent linearity, accuracy, and precision. Furthermore, the practical application of this assay in a tissue distribution study revealed a non-uniform accumulation pattern of imidacloprid, with the highest concentrations observed in the muscle and intestine, and the lowest in the heart. These findings provide a powerful tool and essential empirical data for further biodistribution investigations and environmental risk assessments of trace-level contaminants in micro-gram level biological samples.
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PubMed
高影响因子
MOLECULES
·
2020
·Vol. 25
·期 9
·2149
·
IF 3.267
Xu Yu,Fei Ma,Liangxiao Zhang,Peiwu Li
Rapeseed (Brassica napus L.) is rich in phenols, vitamins, carotenoids, and mineral elements, such as selenium. Additionally, it contains the active ingredients sulforaphane and indole-3-carbinol, which have been demonstrated to have pharmacological effects. In this study, sulforaphane and indole-3-carbinol were extracted and quantified from rapeseeds using quick, easy, cheap, effective, rugged and safe (QuEChERS) method coupled with ultra high performance liquid chromarography tandem mass spectrometry (UHPLC-MS/MS). The major parameters for extraction and purification efficiency were optimized, including the hydrolysis reaction, extraction condition and type and amount of purification adsorbents. The limit of detection (LOD) and the limit of quantification (LOQ) for sulforaphane were 0.05 μg/kg and 0.15 μg/kg, and for indole-3-carbinol were 5 μg/kg and 15 μg/kg, respectively. The developed method was used to successfully analyze fifty rapeseed samples. The QuEChERS coupled with UHPLC-MS/MS simultaneously detect sulforaphane and indole-3-carbinol in vegetable matrix and evaluate the quality and nutrition of rapeseed samples.Keywords:sulforaphane;indole-3-carbinol;QuEChERS;quantification;UHPLC-MS/MS
研究领域:
农业化学
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分析化学
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食品科学
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DOI
PubMed
高影响因子
Journal of Pharmaceutical Analysis
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2020
·
IF 2.673
Siqi Ren,Jingjing Liu,Yunwen Xue,Mei Zhang,Qiwei Liu,Jie Xu,Zunjian Zhang,Rui Song
Saikosaponins (SSs) are the main active components extracted from Bupleuri Radix (BR) which has been used as an important herbal drug in Asian countries for thousands of years. It has been reported that the intestinal bacteria plays an important role in the in vivo disposal of oral SSs. Although the deglycosylated derivatives (saikogenins, SGs) of SSs metabolized by the intestinal bacteria are speculated to be the main components absorbed into the blood after oral administration of SSs, no studies have been reported on the characteristics of SGs for their intestinal absorption, and those for SSs are also limited. Therefore, a rapid UHPLC-MS/MS method was developed to investigate and compare the apparent permeability of three common SSs (SSa, SSd, SSb 2 ) and their corresponding SGs (SGF, SGG, SGD) through a bidirectional transport experiment on Caco-2 cell monolayer model. The method was validated according to the latest FDA guidelines and applied to quantify the six analytes in transport medium samples extracted via liquid-liquid extraction (LLE). The apparent permeability coefficient ( P app ) determined in this study indicated that the permeability of SGs improved to the moderate class compared to the corresponding parent compounds, predicting a higher in vivo absorption. Moreover, the efflux ratio (ER) value demonstrated an active uptake of SSd and the three SGs, while a passive diffusion of SSa and SSb 2 .
研究领域:
药理学
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药剂学
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分析化学
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中药学
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DOI
PubMed
高影响因子
JOURNAL OF SEPARATION SCIENCE
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2022
·Vol. 45
·期 15
·2977-2986
·
IF 3.614
Minhan Huang,Ting Zhou
Pseudotargeted analysis combines the advantages of untargeted and targeted metabolomics methods. This study proposed a comprehensive pseudotargeted metabolomics method based on two-phase liquid extraction using ultra-high-performance liquid chromatography-tandem mass spectrometry. Two-phase liquid extraction, composed of both aqueous and organic phases, extracted a wide range of metabolites from polar to nonpolar in plasma samples. Besides, the two phases were combined and detected in a single injection to save analytical time. A total of 486 potential metabolites were detected by the developed approach. Compared with the conventional methanol-based protein precipitation method, the two-phase liquid extraction method significantly increased the metabolite coverage by 20.29%. Besides, the proposed pseudotargeted metabolomics method exhibited higher sensitivity and better repeatability than the untargeted method. Finally, we applied the established pseudotargeted method to the metabolomics study of depressive rats and screened 53 differential variables. Sixteen determined differential metabolites were mainly in four metabolic pathways including glycerophospholipid, arachidonic acid, sphingolipid metabolisms, pentose and glucuronate interconversions. The results indicated that the pseudotargeted method based on two-phase liquid extraction broadened the metabolite coverage with good sensitivity and repeatability, exhibiting significant potential for discovering differential metabolites in metabolomics studies.
研究领域:
分析化学
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代谢组学
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医学
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产品关联
DOI
PubMed
高影响因子
EUROPEAN FOOD RESEARCH AND TECHNOLOGY
·
2023
·Vol. 249
·期 8
·2017-2027
·
IF 3.3
Han Zai-Gang,Zhang Lingli,Qi Chao,Shi Qing,Min Jun Zhe
The detection and analysis of α-dicarbonyl compounds (α-DCs) in food can guide the daily diet of patients with various chronic diseases. However, these compounds have poor stability, lack color-generating groups, and have low ionization efficiency. Therefore, it is difficult to monitor them. We established a new simple and sensitive method for the simultaneous determination of four α-DCs, including glyoxal (GO), methylglyoxal (MG), 2,3-butanedione (DMGO), and 3-deoxyglucosone (3-DG) in beer by ultra-high-performance liquid chromatography–tandem mass spectrometry (UHPLC-MS/MS) with pre-column derivatization using 3-benzyl-2-oxo-4λ 3 -thiazolidine-4-carbohydrazide (BOTC), a novel MS probe for targeted identification of carbonyl compounds. α-DCs were derivatized with BOTC at 60 °C for 60 min, and the gradient analysis was carried out on a CSH C18 (2.1 mm × 50 mm; 1.7 μm) column for 5 min with a mobile phase A of 0.1% formic acid (FA) in water and mobile phase B of 0.1% FA in acetonitrile. The linearity range of this method was 0.39–500 μM ( R 2 ≥ 0.9995). The limits of detection (LOD) were in the range of 13–50 fmol. The average recoveries of α-DCs were 95.15–101.67%. This method was successfully applied to the detection of α-DCs in beer; the content of 3-DG was the highest, several hundred times higher than that of GO, MG, and DMGO, and the difference was significant. This new BOTC derivatization-based UHPLC-MS/MS method for the simultaneous detection of four α-DCs in beer is highly sensitive and can be used for the detection of α-DCs in alcoholic beverages. Graphical abstract
研究领域:
食品科学
·
分析化学
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高影响因子
危险品化学品经营许可证（带存储）