JOURNAL OF CHROMATOGRAPHIC SCIENCE
·
2021
·Vol. 59
·期 6
·510-520
·
IF 1.618
Xue Ying,Wang Ziteng,Cai Weimin,Tian Xin,Liu Shuaibing
Ticagrelor is recommended for management of patients with acute coronary syndromes. Green tea is one of the most popular beverages in China and around the world. Their concomitant use is unavoidable. In this study, a selective and sensitive liquid chromatography–tandem mass spectrometry method for the simultaneous determination of plasma concentrations of ticagrelor, its two metabolites and four major constituents of tea polyphenols (TPs) in rats was developed for co-administration study of ticagrelor and TPs. Diazepam was used as internal standard (IS). Plasma samples were extracted employing a liquid–liquid extraction technique. Chromatographic separation was carried out on a Kinetex C18 column (2.1 × 75 mm, 2.6 μm) by gradient elution using 0.1% formic acid in water, acetonitrile and methanol. Seven analytes and IS were detected by a mass spectrometer with both positive and negative ionization by multiple reaction monitoring mode. The method was fully validated to be reliable and reproducible in accordance with food and drug administration (FDA) guidelines on bioanalytical method validation. The method was then successfully applied for pharmacokinetic study of ticagrelor, its two metabolites and four major constituents of TPs in rat plasma after oral administration of ticagrelor and tea polyphenol extracts.
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JOURNAL OF SEPARATION SCIENCE
·
2019
·Vol. 42
·期 16
·2668-2678
·
IF 2.516
Ruijuan Liu,Fang Zhao,Jingyao Wei,Pei Yu,Ji Zhang,Yueqin Wang,Zeyun Li,Jiali Zhang,Xiaojian Zhang,Xin Tian
Ribonucleic acid N 6 -methyladenosine methylation plays an important role in a variety of biological processes and diseases. Acetaminophen-induced hepatotoxicity is one of the major challenges faced by clinicians. To date, the link between N 6 -methyladenosine and acetaminophen-induced hepatotoxicity has not been studied. In this study, a simple ultra high performance liquid chromatography with tandem mass spectrometry method was developed for the simultaneous determination of five nucleosides (adenosine, uridine, cytidine, guanosine, and N 6 -methyladenosine) in messenger ribonucleic acid. After enzymatic digestion of messenger ribonucleic acid, the nucleosides sample was separated on an Acquity UPLC column with gradient elution using methanol and 0.02% formic acid water, and detected by a Qtrap 4500 mass spectrometer with an electrospray ionization mode. The method was validated over the concentration ranges of 4–800 ng/mL for adenosine, uridine, cytidine, and guanosine and 0.1–20 ng/mL for N 6 -methyladenosine. It was successfully applied to the determination of N 6 -methyladenosine levels in liver messenger ribonucleic acid in an acetaminophen-induced hepatotoxicity mouse model and a control group. This study offers a method for the determination of nucleoside contents in epigenetic studies and constitutes the first step toward the investigation of ribonucleic acid methylation in acetaminophen-induced hepatotoxicity, which will facilitate the elucidation of its mechanism.
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2021
·
IF 3.205
Xiangling Feng,Yufeng Ding,Peng Zhang,Qiang Fu,Li Zhang,Heng Zheng
Dacomitinib, an irreversible pan-ErbB tyrosine kinase inhibitor targeting the human epidermal growth factor receptor, is used for the treatment of metastatic non-small cell lung cancer. To facilitate the investigations on its metabolism and other relevant studies, based on high-performance liquid chromatography-tandem mass spectrometry (HPLC–MS/MS), a rapid and sensitive bioanalytical technique was established and fully validated for simultaneous quantification of dacomitinib and its main metabolite in human plasma. The plasma samples were treated with acetonitrile containing 0.1% formic acid and the liquid supernatant was collected, dried and dissolved in methanol-water-formic acid (200:800:1, v/v) before injection. The chromatographic separation was performed on an ACE Excel C 18 column (2.1 mm × 50.0 mm, i.d., 5 μm) by gradient elution with a mixture of buffer (5 mM ammonium acetate in 0.1% formic acid) and acetonitrile, serving as the mobile phase, with an overall run time of 4 min. Dacomitinib, O-desmethyl dacomitinib and IS were subsequently detected on an AB QTRAP 5500 mass spectrometer in positive ion and multiple reaction monitoring modes at the precursor-to-product transitions of m / z 470.4 → 385.0, m / z 456.0 → 370.9 and m / z 480.2 → 385.1, respectively. The accuracy and precision of determinations were guaranteed within the concentration ranges of 0.25–100 ng/mL for dacomitinib and 0.20–80 ng/mL for O-desmethyl dacomitinib. The intra- and inter-assay accuracy ranged from 92.00% to 104.50% and the intra- and inter-assay precision was less than 8.20% for each analyte. The method was validated and the relevant parameters, including selectivity, interference among analytes and internal standard, carry-over effect, dilution integrity, extraction recovery, matrix effect, and stability, all satisfied the requirements formulated by the US Food and Drug Administration and the European Medicines Agency. The clinical applicability of the fully-validated method was evaluated in medicated samples from patients on dacomitinib.
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BIOMEDICAL CHROMATOGRAPHY
·
2016
·Vol. 30
·期 11
·1796-1806
·
IF 1.729
Junjun Ni,Li Xu,Wei Li,Lijun Wu
Easy-to-use early cancer detection methods based on metabolomics using serum samples have been developed recently. Among metabolites, amino acids and acylcarnitine are two of the most suitable candidates for diagnosing lung cancer. The purpose of the present study was to develop a novel, sensitive and specific liquid chromatography–tandem mass spectrometry (LC–MS/MS) method to simultaneously determine 13 amino acids and 8 acylcarnitines in lung cancer patients in serum. After derivatization, the 21 analytes were separated using a C 18 column with gradient elution program in 14 min, obtaining recovery within 90.4–113.8% and precision within 0.3–14.8%. The method was successfully applied in concentration determination of lung cancer patients and healthy controls. The results showed that the serum concentration of lung cancer patients were significant from those of healthy controls.
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XENOBIOTICA
·
2024
·
IF 1.3
Li Shao,Jiajia Mo,Qinlong Xu,Guangwei He,Chunyu Xing,Zhaoxing Chu
HY-072808 is a novel phosphodiesterase 4 inhibitor clinically used for topical atopic dermatitis treatment. Cytochrome P450 enzymes are involved in transforming it into major metabolite ZZ-24. An efficient UPLC–MS/MS method was established to detect HY-072808 and ZZ-24 in plasma and skin tissues of minipigs.One-step protein precipitation was performed with acetonitrile. Subsequently, elution was served with a methanol and water gradient containing 0.1% formic acid for 3.5 min. The plasma and skin tissue concentrations of HY-072808 and ZZ-24 showed good linearity from 0.200 to 200 ng/mL.The experimental minipigs exhibited low systemic exposure and bioavailability of 3.1–7.6% after transdermal application of 1–4% HY-072808 ointment. Multiple topical administrations over seven consecutive days showed a minor accumulation in systemic exposure, with accumulation factors of 2.3 and 4.0 for HY-072808 and ZZ-24, respectively.The distribution of HY-072808 ointment among different cortical layers in minipigs was studied for the first time. Following transdermal application of 2% HY-072808 ointment, the concentration in plasma and skin tissues in the order of epidermis > dermis > subcutaneous tissue ≈ subcutaneous muscle ≈ plasma; at 48 h after the administration, the epidermis and dermis still had a high concentration of the drug.
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Analytical Methods
·
2014
·Vol. 6
·期 9
·2998-3008
·
IF 1.938
Guanghui Liu,Wei He,Hao Cai,Xiuman Sun,Waner Hou,Manna Lin,Zhiyong Xie,Qiongfeng Liao
A rapid and sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed to simultaneously determine berberine, palmatine, coptisine, epiberberine and jatrorrhizine in rat plasma, using tetrahydropalmatine as an internal standard. The separation of the five compounds was carried out on a C18 column using a mobile phase consisting of acetonitrile and water (containing 5 mmol ammonium acetate adjusted to pH 5.0 with formic acid). The detection was performed in the multiple reaction monitoring (MRM) mode via the electrospray ionization (ESI) source operating in the positive ionization mode. Linear calibration curves were obtained over the concentration range of 0.20–200.0 ng ml−1 for berberine, and 0.20–100.0 ng ml−1 for palmatine, coptisine, epiberberine and jatrorrhizine. The accuracy, precision and extraction recovery of the five analytes were all satisfactory. The validated method was successfully applied to study the pharmacokinetic differences of the five protoberberine-type alkaloids after the oral administration of Rhizoma coptidis (RC) and Jiao-Tai-Wan (JTW) extract. It was found that the Tmax values of the five ingredients in the JTW extract were significantly increased (P < 0.05) when compared with those in RC. In addition, the AUC0–t of palmatine, coptisine and epiberberine were significantly increased (P < 0.05).
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PHYTOCHEMICAL ANALYSIS
·
2025
·
IF 2.6
Peng Yang,Hu-Dong Lv,Jie Wu,Fang Long,Jing Zhou,Cheng-Ying Wu,Jin-Di Xu,Shan-Shan Zhou,Qing-Ling Xiao,Song-Lin Li,Hong Shen
Introduction The role of macromolecular components in traditional Chinese medicines (TCMs) decoction remains poorly understood, primarily because of their structural complexity and limited systemic bioavailability. In the modernization of TCMs' decoctions, macromolecular components are often removed as “poor bioavailable impurities” by ethanol precipitation that might attenuate the efficacy thereof. Purpose A novel strategy integrating LC–MS-based serum pharmacochemistry, network pharmacology, and pharmacodynamics was developed to reveal the role of macromolecular components in TCMs' decoction, using Qi-Huo-Yi-Fei decoction (QH) treating chronic obstructive pulmonary disease (COPD) as a case study. Materials and Methods QH was separated into macromolecular components (QH-M) and small molecular components (QH-S) by ethanol precipitation. The absorbed components of QH and QH-S in serum were qualitatively and semiquantitatively analyzed by UPLC-QTOF-MS/MS. The differences in targets and pathways of the absorbed components were predicted by network pharmacology analysis. The therapeutic effects on pulmonary function, histopathology, and inflammation of QH, QH-S, and QH-M were comparatively investigated on a COPD rat model. Result A total of 103 components were identified in QH and QH-S, whereas 86 and 72 were detectable in QH- or QH-S-treated serum, respectively. The highest levels of absorbed components appeared from 15 to 60 min for QH-S and at 15 min for QH. The concentrations of most absorbed components of QH were twofold higher than those of QH-S. Their protein–protein interaction (PPI), herb–component–target networks, and GO/KEGG enrichment pathways were quite different, mainly in inflammatory, immunity, and cell apoptosis processes. QH-M improved pulmonary function, histopathology, and inflammatory infiltration, mainly on FVC ( p < 0.05), thickness/external diameter ( p < 0.01), Wac/Pbm ( p < 0.01), TNF-α ( p < 0.01), and IL-17 ( p < 0.05). Meanwhile, QH was more effective than QH-S, mainly on FEV0.3/FVC, MAN, GC/CC, TNF-α, and IL-17. Conclusion QH-M was not only effective independently on COPD but also showed integrative effects with the coexisting QH-S in improving their absorption, thus strengthening the component–target interactions, and consequently contributing to the COPD therapeutic effects of QH. Therefore, it was confirmed that QH-M was essential for QH's COPD therapy and should not be removed during the modern preparation development.
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FOOD CHEMISTRY
·
2025
·
IF 9.8
Zi-Ling Li,Da-Jin Yang,Jia-Qi Zhao,Wen-Jie Sun,Jie Gao,Shu-Feng Song,Hou-Jun Xu,Hai-Jie Li,Fa-Ming Tian,Man-Man Wang
A novel magnetic nanoporous carbon (Fc-Fe/Ni@MPC) was fabricated from ferrocene contained metal-organic framework (MOF) and employed as multifunctional QuEChERS adsorbent for determination of triazine herbicides in various fruit and vegetable samples before LC-MS/MS. The prepared Fc-Fe/Ni@MPC not only maintained the original ordered morphology from MOF precursor, but also exhibited high graphitization and good superparamagnetism through pyrolysis. This sorbent afforded adsorption capacity of 1163.25 mg/g, 157.83 mg/g, 157.69 mg/g and 25.10 mg/g towards chlorophyll, lycopene, β -carotene and lutein via hydrophobic, π-π and hydrogen bonding interactions. The method gave negligible matrix effects of −14.2 % ∼ 10.8 %, low detection limits of 0.001–0.04 μg/kg and satisfactory recoveries of 80.2 %–112 % in orange, citrus, apple, watermelon, tomato, carrot and lettuce samples, when performing 2 mg of this single sorbent within just 15 s. This work revealed the prospect of Fc-Fe/Ni@MPC as versatile and efficient QuEChERS adsorbent for pretreatment of triazine herbicides in large kinds of pigment-rich food samples.
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BIOMEDICAL CHROMATOGRAPHY
·
2024
·Vol. 38
·期 12
·e6034
·
IF 1.8
Feng Chen,Huanhuan Li,Xiaoxia Yang,Ziwei Deng,Hongqiang Wang,Zhihua Shi,Chengfeng Qiu
To facilitate clinical therapeutic drug monitoring (TDM) of polymyxin B (PB) and polymyxin E (PE), we developed and validated a simple LC–MS/MS method for simultaneous determination of PB (including polymyxin B1 (PB1), polymyxin B2 (PB2), polymyxin B3 (PB3) and isoleucine-polymyxin B1 (ile-PB1)) and PE (including polymyxin E1 (PE1) and polymyxin E2 (PE2)) in human plasma. PB or PE was extracted from 20.0 μL plasma using a 5% (v/v) formic acid acetonitrile solution and separated on a BEH-C18 column (2.1 × 100 mm, 1.7 μm) with a mobile phase consisting of 0.8% formic acid aqueous solution and 0.2% formic acid acetonitrile solution. Gradient elution was performed over 5.5 min at a flow rate of 0.250 mL/min. Quantitative analysis was conducted in positive ion scanning mode by electrospray ionization and multiple reaction monitoring. The method validation was conducted based on bioanalytical method validation guidance, including specificity, calibration curve, precision, accuracy, recovery, matrix effect, stability and dilution integrity and all of the results satisfied the requirements. The method was simple, robust and high-throughput and is currently being used to provide a TDM service to enhancing therapeutic efficacy and safety use of the PB and PE.
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Marine Drugs
·
2026
·Vol. 24
·期 6
·215
·
IF 5.7
Xiaochen Niu,Jun Zhao,Deqi Ding,Wei He,Guanhua Du,Jiejie Hao,Jianchun Zhao
LY104 (previously designated as B7) is a selective phosphodiesterase 4 inhibitor with promising activity against chronic obstructive pulmonary disease. We previously reported its single-dose pharmacokinetics and tissue distribution in rats. In the present study, a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated for the simultaneous quantification of LY104 and its major metabolite M1 in rat plasma following ICH M10 guidelines. The method showed excellent linearity over 20–1200 ng/mL for both analytes, with retention times of 2.85 min (LY104) and 3.22 min (M1). Using this method, we extended our previous work in several directions. Re-analysis of previously published single-dose pharmacokinetic and tissue distribution data revealed no significant sex differences for LY104. Newly generated multiple-dose studies (1 mg/kg daily for 7 days) demonstrated no accumulation of LY104 or M1. The pharmacokinetic profile of M1 was quantified for the first time. Comprehensive in vitro investigations included plasma and liver microsomal stability, plasma protein binding, and excretion studies. This systematic preclinical pharmacokinetic characterization of LY104 and M1, incorporating re-analysis of existing data with sex stratification, newly generated multiple-dose and metabolite data, excretion studies, and comprehensive in vitro investigations, provides useful information to support further drug development and clinical trial design.
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MICROCHEMICAL JOURNAL
·
2018
·
IF 2.746
Guihua Gao,Yanyan Xing,Tingting Liu,Jian Wang,Xiaohong Hou
Four water stable metal-organic frameworks (MOFs), MIL-101(Cr), MIL-100(Fe), MIL-53(Al), and UiO-66(Zr), were used as adsorbents for concentration of four androgens and progestogens from water. The adsorption abilities of target analytes on the four MOFs were investigated by experimental and molecular simulation strategies, and UiO-66(Zr) was ultimately selected as the sorbent to develop a porous membrane protected micro-solid-phase extraction (μ-SPE) method for simultaneous extraction androgens and progestogens in environmental water samples followed by LC-MS/MS detection. Several variables affecting the extraction efficiency were systematically investigated, including pH, salt concentration, extraction time, kind of desorption solvent, and desorption time. Under the optimized conditions, excellent linearity was obtained in the range of 20.32–2032 ng/L for T, 10.24–1024 ng/L for P, 7.624–762.4 ng/L for TP , and 8.376–837.6 ng/L for MPA . Limits of detection (LODs) and limits of quantification (LOQs) were 10 ng/L and 20 ng/L for T, 4.0 ng/L and 10 ng/L for P, 2.0 ng/L and 7.0 ng/L for TP, and 3.0 ng/L and 8.0 ng/L for MPA, respectively. The recoveries were ranged from 80.5% to 102.4%. Furthermore, the μ-SPE device could be used for at least 10 extractions (RSD < 10.0%). Meanwhile, comparison was made with solid-phase extraction, and the developed method was demonstrated to be a convenient and eco-friendly pretreatment method for water samples.
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PHYTOMEDICINE
·
2022
·
IF 6.656
Yu Du,Chang Li,Shouchao Xu,Jiehong Yang,Haitong Wan,Yu He
Background Astragali Radix-Safflower combination (ARSC) is widely utilized in clinic to treat cerebral ischemia/reperfusion injury (CI/RI). Whereas, there is no in-depth research of the pharmacokinetics (PK) and pharmacodynamics (PD) analysis of ARSC after intragastric administration in rats with CI/RI. Purpose The purpose of this research is to investigate the PK characteristics of eight active ingredients (astragaloside IV, calycosin , calycosin-7-O-β-glucoside, formononetin , ononin , hydroxysafflor yellow A, syringin and vernine) of ARSC, and the regulation of neurotransmitters disorders, revealing the pharmacodynamic substance basis and the mechanism of ARSC in treating CI/RI from the molecular level. Methods We established a new method which based on blood-brain dual channel microdialysis (MD) coupled with liquid chromatography-tandem mass spectrometry (LC-MS/MS) to continuously gather, and determine the components of ARSC and neurotransmitters related to CI/RI in vivo . The collected data were analyzed by sigmoid-E max function. The neurotransmitters primarily regulated in CI/RI rat were discussed by principal component analysis and the compound most associated with total pharmacodynamics was chosen by partial least squares regression . Results The validated LC-MS/MS method had specificity and selectivity to simultaneously analyze the concentration of eight active components of ARSC extract and five neurotransmitters of CI/RI rats. The recovery rates of brain MD probe and blood MD probe were stable within six hours. The MD probes recovery rates decreased with the increase of flow rates, but the solution concentration had little effect on the probes recovery rates. It was feasible to correct the recovery rates of probes in vivo by using reverse dialysis method. All eight active ingredients of ARSC could pass across the blood brain barrier after CI/RI. ARSC regulated the release of glutamate (Glu), γ-aminobutyric acid (GABA), dopamine (DA), 5-hydroxytryptamine (5-HT) and aspartic acid (Asp). Notably, astragaloside IV and hydroxysafflor yellow A might have better regulatory effect on neurotransmitters in comparison with other six measured components of ARSC, and Glu was the neurotransmitter mainly regulated in CI/RI rats. Conclusion The ARSC was able to treat CI/RI through ameliorating neurotransmitters disorders. There was a hysteresis between the peaked drug concentration and maximum therapeutic effect of ARSC. The drug effective concentrations range of ASIV, calycosin, calycosin-7-O-β-glucoside, syringin and vernine in blood microdialysate and calycosin, syringin, vernine in brain microdialysate were narrow, which need be paid attention in clinical use.
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