Separation Science Plus
·
2026
·Vol. 9
·期 5
·e70227
·
IF 2.7
Qingqing Xiao,Chengsi Cao,Zuding Wang,Fei-fei Wang,Shizhi Jiang,Ting Lei
Pinus yunnanensis cones are a rich source of bioactive compounds; yet, the systemic exposure and mechanistic basis of their anti-breast cancer activity remain unclear. Herein, we systematically identify the systemically absorbed components of P. yunnanensis cone extract and elucidate its anti-breast cancer mechanisms using an integrated analytical and computational approach. An optimized ultra-high performance liquid chromatography–tandem mass spectrometry (UHPLC–MS/MS) method was developed to overcome severe matrix interference and insufficient sensitivity, facilitating the rapid identification of active constituents in the crude extract. UHPLC–MS/MS-based analysis of rat plasma and feces revealed 16 (14 prototypes and 2 metabolites) and 12 (10 prototypes and 2 metabolites) systemically absorbed components, respectively, derived from 28 identified compounds. Subsequent network pharmacology combined with molecular docking validation was used to screen the anti-breast cancer active components, core targets, and key pathways. Integrated network pharmacology predicted coniferaldehyde, phyllanflexoid A, 3′,4′,5,5′,6,7-hexamethoxyflavone, dihydrocaffeic acid, usnic acid, and 7-oxodehydroabietic acid, as core components, targeting TP53, STAT3, PIK3R1, SRC, and PIK3CA and involving key pathways such as VEGF signaling pathway, aldosterone-regulated sodium reabsorption, prolactin signaling pathway, PD-L1/PD-1 checkpoint pathway in cancer, and ErbB signaling pathway. This study establishes a robust UHPLC–MS/MS platform for the quality control of P. yunnanensis cones and provides critical insights into their translational potential for anti-breast cancer drug development and advancing separation science applications in natural product research.
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高影响因子
FOOD CHEMISTRY
·
2020
·
IF 6.306
Xu Yu,Li Yu,Fei Ma,Peiwu Li
In the present work, a rapid, accurate and cost-effective method has been developed for the simultaneous quantification of phenolic compounds in oil using mixed-mode solid-phase extraction (SPE) coupled with chemical labeling UHPLC-MS/MS. Mix-mode SPE weak cation cartridges were selected to enrich and purify phenolic compounds in oil, and hydroxyl moiety was dansylation as stable-isotope internal standard. The major parameters that affected the extraction and chemical labeling efficiency were investigated, and the method was fully validated. The limit of quantifications and the limit of detections were 0.002 µg kg −1 ~ 0.10 µg kg −1 and 0.006 µg kg −1 ~ 0.30 µg kg −1 , respectively. The recoveries were 61.2% ~ 129.3% with intra-day and inter-day precision less than 12%. The results for 38 rapeseed oils revealed that 14 phenolic compounds, including canolol, phenolic acids, phenolic alcohols, tyrosol and vanillin from trace levels to relatively high content.
研究领域:
分析化学
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食品科学
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PubMed
高影响因子
Bioanalysis
·
2026
·
IF 2.1
Sijia Li,Jiameng Xie,Fan Xia,Tingting Yang,Fangyue Zheng,Liyan Miao,Chenrong Huang
Background Bruton’s tyrosine kinase inhibitors (BTKis, ibrutinib, zanubrutinib, orelabrutinib) are key targeted therapies for B-cell lymphomas, but interindividual variability and adverse reactions limit their use. Metabolized by CYP3A, co-medications or hepatic dysfunction cause plasma fluctuations, necessitating therapeutic drug monitoring (TDM). Cerebrospinal fluid (CSF) distribution is also critical for CNS lymphoma treatment.Objective To develop and validate a UHPLC-MS/MS method for simultaneous quantification of three BTKis and one metabolite in human plasma and CSF to support TDM.Methods After protein precipitation with methanol, samples were analyzed on an ACQUITY HSS T3 column with a 3-min gradient at 0.3 mL/min and ESI (+) MRM. Mobile phase: water–acetonitrile–formic acid–ammonium acetate (1 M) (950:50:1:1, A) and (50:950:1:1, B).Results The method showed excellent selectivity and linearity (r > 0.997) over 1–200 ng/mL (ibrutinib, zanubrutinib, ibrutinib metabolite) and 5–1000 ng/mL (orelabrutinib) in both matrices. Recoveries were 89.4–103.8%, matrix factors 0.93–1.06, and precision CV ≤8.5%. Stability was confirmed. The method was applied to 34 clinical samples (25 plasma, 9 CSF) from 20 patients.Conclusion This method detects four BTK-related analytes in plasma/CSF with a 3-min run time, evaluation of hemolytic/lipemic matrices, and clinical validation, increasing throughput, reducing costs, and broadening applicability, providing preliminary feasibility data for clinical TDM.
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高影响因子
Food Chemistry-X
·
2025
·
IF 8.2
Yuxin Wang,Jin Liu,Suzhen Li,Jizhen Fu,Xiaowen Wang,Li Li,Xu Jing
The widespread use of triazole fungicides has raised concerns over residual. This study presents an automated, environmentally friendly, simple, and efficient method for detecting triazole fungicides in food samples, utilizing high-throughput liquid processing, dispersive liquid-liquid microextraction, and ultra-high-performance liquid chromatography-tandem mass spectrometry. The automated liquid handling workstation was employed to automate the whole sample pre-treatment process. Fatty acid, bio-based solvent, and saturated sodium chloride solution were used as the extractant, dispersant, and demulsifier, respectively. The whole operation process obviated the use of toxic reagents and eliminated the need for time-consuming centrifugation. The linear ranged from 0.01 to 1 μg L −1 with limits of detection and quantification of 0.003 μg L −1 and 0.01 μg L −1 , respectively. Ten triazole fungicides were successfully detected in food samples with recoveries of 70.1 %–105.7 %. The automation of dispersive liquid-liquid microextraction demonstrates huge potential for broad applicability within the field of food safety testing.
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Food Chemistry-X
·
2025
·
IF 8.2
Yuanfeng Zhao,Jingrui Zhou,Wenju Luo,Lingling Jiang,Fuzhan Song,Jiang Ran,Haoxiang Xu,Lu Lei,Rong Ai,Bo Yu
This study investigated breed-specific flavor characteristics in Guanling (GL), Sinan (SN), and Simmental-crossbred (XZ) cattle using UHPLC-MS/MS and GC × GC-TOF MS. Specifically, XZ had 73 and 48 differential metabolites compared to GL and SN, respectively, whereas GL and SN showed 31 discriminated metabolites. Notably, these differences were linked to flavor-related metabolic pathways, particularly beta-alanine, histidine, glutathione, and purine metabolism. Regarding the composition of volatile organic compounds (VOCs), GL displayed a higher ketone content (18.58 %), whereas XZ was enriched in alcohol (56.25 %). Key VOCs with the highest flavor contributions across all breeds were 2,3-Butanedione, (E)-2-nonenal, 2-ethyl-1-hexanol, and (E)-2-octenal. However, dimethyl sulfide contributed significantly to GL and SN flavors but not to XZ. Collectively, the 49 differential VOCs led to aroma profiles of breeds varied in “sweet”, “fruity”, “nutty”, and “waxy” characteristics. This comprehensive analysis of non-volatile metabolites and flavor-related VOCs revealed breed-specific profiles and crossbreeding effects, providing insights for improving meat quality.
研究领域:
食品科学
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畜牧学
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分析化学
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代谢组学
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风味化学
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PubMed
高影响因子
RSC Advances
·
2024
·Vol. 14
·期 46
·34261-34269
·
IF 3.9
Min Xie,Jun Xu,Dan Fei,Ye-Lan Guang,Yao-Min Zhou,Fan Li,Li-Zhen Hu
An improved QuEChERS method combined with Multi-Plug Filtration Cleanup (m-PFC) clean-up procedure was developed for the simultaneous determination of 16 different sulfonamides in forage grasses using ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS). The forage grass sample was extracted with 0.1 mol L−1 Na2EDTA-Mcllvaine buffer and acetonitrile solution, purified by the Navo U-QuE column tube, separated by Agilent ZORBAX Eclipse Plus C18 column, and analyzed by MRM (multiple reaction monitoring) mode and the internal standard method was utilized for quantification. The 16 different sulfonamides display good linearity within the range of 0.5–50 μg L−1 (R2 > 0.9967), the limit of detection was 0.02–0.5 μg kg−1, and the limit of quantification was 0.05–1.0 μg kg−1. Under the additive amounts of 1, 2, and 10 μg kg−1, the recoveries were in the range of 72.3–116.9%, and the relative standard deviation was between 1.4% and 10.3%. The presented method showed the advantages of simple operation, excellent selectivity and high sensitivity. It was well-suited for both qualitative and quantitative analyses of sulfonamides in forage grass. Overall, this method provided a scientific basis for risk assessment, enforcement of quality and safety standards, and detection of sulfonamide residues in forage grass for import and export.
研究领域:
分析化学
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兽医学
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食品安全
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药物分析
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高影响因子
MICROCHEMICAL JOURNAL
·
2024
·
IF 4.9
Di Jiao,Zhen-Jie Qian,Yu Wang,Xi Zeng,Yu-Xin Zhong,Lin Luo,Yong-Xin He,Yi-Na Lu,Hong-Tao Lei,Zhen-Lin Xu
Gizzerosine is a biogenic amine in feeds with a physiological toxicity 1,000 times that of its precursor, histamine, causing high mortality in poultry. Because feeds containing gizzerosine usually contain high concentrations of histamine, it is of great significance to establish a method for the simultaneous detection of gizzerosine and histamine for feed safety. Herein, we first developed a detection method using 50 % (v/v) acetonitrile(ACN) containing 1 % (v/v) ammonium hydroxide (AH) extraction to synchronously monitor gizzerosine and histamine in feeds and raw materials via UHPLC–MS/MS. Due to the serious positive matrix effect (ME) in existing LC–MS/MS, this study reduced the ME of samples by purifying the extract solution using a mixed-mode cation exchange based solid phase extraction column (MCX-SPE), and simultaneously obtained accurate quantities of 5–500 ng mL −1 gizzerosine and 25–2,500 ng mL −1 histamine. The limit of detection (LOD) values for gizzerosine and histamine were 1.02 ng mL −1 and 3.00 ng mL −1 , respectively, which were approximately 390 and 8,000 times more sensitive than the maximum recommended dosage of gizzerosine (0.4 mg kg −1 ) and limitation standards of histamine (25 mg kg −1 ) in fish meal, respectively. The samples could only be evaluated in 2 h. The average recoveries of the 6 types of feeds and raw materials ranged from 79.73 % to 110.31 % with a relative standard deviation (RSD) ranging from 1.29 % to 13.35 %. The average recoveries of feeds were generally lower than those of raw materials. Our method was efficient, simple, rapid, accurate, sensitive, and suitable for the simultaneous quantitative analysis of gizzerosine and histamine contents in various feeds, which provided technical support for the quality evaluation of feeds.
研究领域:
动物营养学
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食品科学
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分析化学
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高影响因子
Analytical Methods
·
2015
·Vol. 7
·期 19
·8418-8431
·
IF 1.821
Mei Yang,Youning Ma,Wenjun Gui,Yiping Ren,Guonian Zhu,Yihua Liu
Endocrine-disrupting chemicals (EDCs) in the environment have adverse effects on humans and wildlife. A method based on ultrahigh performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) for the determination of 26 EDCs (including five estrogens, eight androgens, three progestogens, six glucocorticoids, two mineralocorticoids and two thyroid hormones) in fish and water was developed. Various experimental parameters that could affect the extraction efficiencies were investigated in detail. The sample was extracted by a modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) method with 20 mL of acetonitrile (for fish) or 5 mL of ethyl acetate (for water), and then cleaned-up using an Oasis HLB SPE (solid-phase extraction) cartridge. The analytes were quantified using an isotope-labelled internal standard and recoveries between 69.1% and 120.5% were obtained. The relative standard deviation of inter- and intra-day analyses for all the compounds was below 20%. The detection limits ranged from 0.01 to 0.98 ng mL−1 for water and 0.01 to 9.04 ng g−1 for fish. For real samples, progesterone and trenbolone were detected in zebrafish (Danio rerio) samples at 5.73 ± 0.21 and 7.45 ± 0.34 ng g−1, respectively. There was no target analyte detected in tap-water samples. The developed method would be useful for monitoring EDC abuse in fishery, potential EDC screening and risk assessment in aquatic toxicology.
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高影响因子
JOURNAL OF HAZARDOUS MATERIALS
·
2023
·
IF 13.6
Jiawen Cheng,Jiping Ma,Shuang Li,Qiaoning Wang,Min Lv,Jinhua Li,Xiaoyan Wang,Hongdan Wang,Lingxin Chen
Hexabromocyclododecanes (HBCDs) have given their adverse effects on environment and human health, and highly sensitive analysis of HBCDs in water is urgent. In this study, a new method for the determination of trace HBCDs in water was established by covalent organic framework (COF) based nylon membrane extraction (ME) coupled with ultrahigh-performance liquid chromatography−tandem mass spectrometry (UHPLC−MS/MS). The COF had been self-assembled onto the nylon membrane in a gentle strategy to fabricate COF nylon membrane. Several important ME parameters including the dosage of COF, pH, eluent condition and salinity were systematically investigated. The limits of detection and quantification were 0.011–0.014 and 0.038–0.047 ng/L for three HBCDs, respectively. The linear ranges were from 0.04 to 20 ng/L, and the relative standard deviations were 5.7–17.8 % (intra-day) and 5.2–14.1 % (inter-day). In addition, density functional theory (DFT) calculations on adsorption energy proved that the introduction of halogen bond (XB) made a key contribution to high extraction efficiency and excellent selectivity of COF nylon membrane for HBCDs. The 500 mL of samples, including tap water and reservoir water, could be extracted only in 23 min. The established method presented highly sensitive for ultra-trace analysis of HBCDs in environmental water.
研究领域:
环境科学
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分析化学
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PubMed
高影响因子
JOURNAL OF SEPARATION SCIENCE
·
2025
·Vol. 48
·期 12
·e70326
·
IF 2.8
Meichen Liu,Yingxia Guo,Jinhe Liu,Zihan Tang,Yufeng Guo,Xintao Liu,Deshan Zhou,Lei Yin,Meiyun Shi
An ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method was developed and validated for the simultaneous determination of fipronil and its three metabolites (fipronil sulfone, fipronil sulfide, and fipronil desulfinyl) in zebrafish tissues. Protein precipitation was employed for sample preparation, followed by chromatographic separation on a C 18 column. The method demonstrated excellent linearity ( r 2 > 0.99) across a range of 0.1–10 ng/mL, with a lower limit of quantification (LLOQ) of 0.1 ng/mL for all analytes. Validation results confirmed acceptable accuracy (−5.0% to 8.9%), precision (0.6%–13.2%), recoveries (86.3%–113.6%), and minimal matrix effects (86.0%–110.6%). When applied to zebrafish exposed to 50 µg/L fipronil for 12 h, the method revealed preferential accumulation of fipronil and fipronil sulfone in liver tissues, while lower levels were detected in muscle tissues. Fipronil sulfide was rarely detected, and fipronil desulfinyl concentrations were below the LLOQ (0.1 ng/mL) in all tested samples. This reliable and sensitive method is well-suited for environmental toxicology studies, pesticide residue monitoring, and ecological risk assessment.
研究领域:
环境毒理学
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分析化学
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农药残留监测
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生态风险评估
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高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2025
·
IF 3.1
Zheming Yu,Yangyang Chen,Fengting Ou,Kui Zeng,Debo He,Lushan Yu
The aim of this study was to develop and fully validate a sensitive and rapid ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method for simultaneous quantification of Dimyristoyl phosphatidylcholine (DMPC) and Dimyristoyl phosphatidylglycerol (DMPG) in biological matrices of rats after intravenous administration of amphotericin B phospholipid complex suspension injection and excipients (DMPC and DMPG). DMPC, DMPG and Loratadine (internal standard, IS) were separated on an Agilent ZORBAX Extend-C18 column (2.1 mm × 50 mm, 3.5 μm particle size) by using gradient elution consisting of isopropanol-acetonitrile (90:10, v/v, 10 mM ammonium formate and 0.1 % formic acid) and water (10 mM ammonium formate and 0.1 % formic acid) at a flow rate of 0.3 mL/min in 4.0 min. Multiple reaction monitoring (MRM) mode was performed to quantify data under monitoring precursor-product ion transitions of m/z 678.9→184.0 (DMPC, ESI+), 665.5→227.2 (DMPG, ESI-) and 383.0→337.1 (loratadine, IS, ESI+), respectively. The method was developed at linearity ranging from 10.0 to 1000 ng/mL for all analytes. The inter-day accuracy of DMPC and DMPG was observed to range between −12.8–12.7 %, while the precision was found to be within 15.0 %. DMPC and DMPG demonstrated stability during sample storage, preparation and analytic procedures. Furthermore, this method was successfully applied in the investigation of the pharmacokinetic profile and tissue distribution of DMPC and DMPG in rats after intravenous administration. Dose-dependent increases were observed for DMPC and DMPG in both areas under the curve (AUC) and maximum plasma concentration (Cmax), demonstrating positive correlations across all tested dose levels. The biological half-lives (t₁/₂) of DMPC and DMPG following intravenous administration of an amphotericin B phospholipid complex suspension were 1.2–3.4 h and 4.6–8.1 h, respectively. However, after intravenous administration of the excipients, their half-lives were 3.5 h and 1.1–2.3 h. The observed prolongation of DMPC's half-life and concomitant shortening of DMPG's half-life are attributed to the distinct physicochemical properties of the nanoparticles.
研究领域:
药物分析
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药代动力学
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分析化学
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药物递送
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纳米医学
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PubMed
高影响因子
MICROCHEMICAL JOURNAL
·
2026
·
IF 5.1
Qing-nan Chen,Yun-e Bai,Yao Ma,Rui Liao,Lu-lu Wang,Shuang Hu,Jian- ping Gao
Latex-bearing plants have gained global attention, but few studies have been reported on Codonopsis pilosula (Franch.) Nannf.( C. pilosula ) latex. In this research, we established a UHPLC-MS/MS method to investigate the constituents in C. pilosula latex. Analysis revealed that the latex of C. pilosula contains alkaloids, terpenoids, and fatty acids, with fatty acids being one of the primary metabolites distinguishing the latex from above-ground (DS) and below-ground (DX) parts of C. pilosula. To evaluate the quality of C. pilosula latex, an approach of dispersive liquid-liquid microextraction with solidification of the floating organic drop (DLLME-SFO) methodology was developed to quantitatively analyze the contents of three fatty acids (palmitic, linoleic, and stearic) in the latex of C. pilosula . The ideal extraction conditions involve injecting 20 μL of dodecanol extractant into a 5 mL 10% NaCl solution at pH 3.0, followed by 20 min at 700 rpm. The three components mentioned above have enrichment coefficients ranging from 48 to 50. The quantification limits were between 0.23 and 0.25 μg/mL, and three components demonstrated good linearity in their respective linear ranges (R 2 > 0.995). The satisfied precision and recovery rates were 1.26 to 8.05% and 92.38 to 101.53%, respectively. By quantitatively analyzing the three fatty acid contents in the latex of C. pilosula , the results showed that palmitic and linoleic acids were able to successfully distinguish the latex of C. pilosula from different parts, which laid the foundation for the quality evaluation of C. pilosula , and provided a reference for the utilization of C. pilosula , a medicinal food source.
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高影响因子
危险品化学品经营许可证（带存储）