BIOMEDICAL CHROMATOGRAPHY
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2023
·
IF 1.8
Qiang Liu,Jin-Zhu Zhao,Fu-Sheng Zhou,Jiong Lan,Qiang Lu,Hong-Can Ren
GFH009 is a potent, highly selective, small molecule that targets and inhibits the activity of the CDK9/cyclin T1 regulatory complex of P-TEFb. This study aimed to develop and validate a highly selective and sensitive ultrahigh-performance liquid chromatography–tandem mass spectrometry (UHPLC–MS/MS) method for precise quantification of GFH009 in rat plasma. This method was subsequently employed for conducting toxicokinetic studies of GFH009 in rats. Plasma was prepared using a simple protein precipitation method by acetonitrile. Chromatographic separation of the analytes was achieved on a BEH C 18 analytical column with a rapid 3.0 min run time and a flow rate of 0.5 ml/min. The calibration curves for plasma samples exhibited excellent linearity over a wide concentration range of 1.0–1,000 ng/ml for GFH009. Intra- and inter-day accuracies were within 92.7–105.7%, and precisions were no more than 6.7%. Furthermore, the analyte demonstrated stability under four different storage conditions, with variations of <15.0%. This study pioneers a methodological innovation by introducing a highly reliable, specific and sensitive analytical method for GFH009 in rat plasma. The successful application of this method in toxicokinetic studies further underscores its significance, offering valuable insights for the methodology of clinical pharmacokinetic research.
研究领域:
药理学
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分析化学
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毒理学
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DOI
PubMed
高影响因子
Bioanalysis
·
2020
·Vol. 12
·期 9
·
IF 2.371
Peng Guo,Qiucheng Liang,Juntao Zheng,Jinmin Chen,Yanping Guan,Liang Ding,Fulin Jiang,Xuewen Chen,Min Huang,Ailan Chen,Guoping Zhong
Aim: Heart failure patients are frequently given comedication of digoxin and diuretics like spironolactone and tolvaptan. A UHPLC–MS/MS assay for determining canrenone (main active metabolite of spironolactone), digoxin and tolvaptan simultaneously should be developed so as to support related drug–drug interaction studies. Results: A UHPLC–MS/MS method for simultaneous determination of these three drugs in human plasma was established and fully verified as per CFDA guidelines. Chromatographic separation was achieved using a 4-min isocratic elution. Mass analyses were performed under positive electrospray ionization mode. The calibration curves were established over 1.0–400.0 ng/ml for canrenone and tolvaptan while over 0.1–40.0 ng/ml for digoxin. Conclusion: The developed method was feasible in detecting concentration and related drug–drug interaction studies.
研究领域:
药理学
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分析化学
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心脏病学
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DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
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2021
·
IF 3.205
Wei-jie Men,Li-yuan Cheng,Meng-ying Chen,Xiao-ying Zhang,Yue Zhang,Kun Zhou
Bufei-Huoxue Capsule (BFHX) was applied to treat chronic obstructive pulmonary disease (COPD) in China. It is composed of Astragali Radix, Paeoniae Radix Rubra, and Psoralea Fructus. A sensitive and reliable ultra-high-performance liquid chromatography-mass spectrometry (UHPLC-MS/MS) method was developed and validated to quantify the eight main bioactive compounds (psoralen, isopsoralen, neobabaisoflavone, corylin, bavachin, astragaloside IV, ononin and formononetin) in rat plasma after oral administration of BFHX. Osthol was used as an internal standard (IS). Plasma samples were pretreated with methanol to precipitate protein. Chromatographic separation was accomplished using Hypersil GOLD TM C18 column (2.1 mm × 100 mm, 1.9 μm) with a gradient elution profile and a mobile phase consisting of (A) 0.1% formic acid in water and (B) acetonitrile and the flow rate was set at 0.2 mL/min. Multiple reaction monitoring (MRM) mode was applied to perform mass spectrometric analyses. All calibration curves were linear (r > 0.9908) in tested ranges. The intra- and inter-day accuracy and precisions of eight compounds at three different concentration levels were within the acceptable limits. The extraction recovery was within the range of 76.4 ∼ 105.2% and the matrix effects were within the range of 88.3 ∼ 115.0% (RSD ≤ 15.6%). The dilution effects were within the range of 90.2 ∼ 114.9%. These 8 compounds were stable under the tested conditions. So the developed method was valid to evaluate the pharmacokinetic study of eight bioactive compounds after oral administration of BFHX.
研究领域:
药理学
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分析化学
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中药学
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药物分析
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色谱-质谱分析
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DOI
高影响因子
CURRENT MICROBIOLOGY
·
2022
·Vol. 79
·期 6
·1-11
·
IF 2.343
Bao Jingjiao,Guo Dengkang,Jin Lei,Li Tiejun,Shi Hui
Vibrio fluvialis is a marine opportunistic pathogen that frequently causes diseases in aquatic animals and humans. V. fluvialis can produce quorum sensing signaling molecules to coordinate cell density-dependent behavioral changes, including N-acyl homoserine lactone (AHL), which acts as a vital mediator of virulence-associated gene expression. Currently, several AHL molecules in V. fluvialis have been detected via biological and physicochemical methods, although different detection approaches have generated diverse AHL profiles. Here, we describe the AHL-producing bacterium, V. fluvialis BJ-1, which was isolated from marine sediments from the East China Sea. V. fluvialis BJ-1 could stimulate AHL-mediated β-galactosidase synthesis of the biosensor Agrobacterium tumefaciens NTL4 (pZLR4) but could not induce violacein production in the AHL reporter strain, Chromobacterium violaceum CV026. This bacterial isolate exhibited strong AHL-producing activity at low cell density; however, the AHL activity declined when population density remained at high levels. Analysis of the AHLs by Ultra-High-Performance Liquid Chromatography tandem Mass Spectrometry demonstrated that V. fluvialis BJ-1 produced five different AHL signaling molecules, including two linear chain AHL products (C 8 - and C 10 -HSL), and three β-carbon-oxidative AHL products (3-O-C 8 -, 3-O-C 10 - and 3-O-C 12 -HSL). Significantly, the present study is the first to accurately define the AHL profile of marine V. fluvialis . In future, the coupling of UHPLC to ESI–MS/MS is expected to be utilized for the accurate determination of AHL profiles in marine Vibrio .
研究领域:
微生物学
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海洋生物学
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分析化学
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DOI
PubMed
高影响因子
ANALYTICAL CHEMISTRY
·
2024
·
IF 6.7
Lyuye Zhang,Weibing Zhang,Hailin Wang
The dynamic landscape of cellular nucleotides/nucleosides associated with RNA metabolism, particularly in diseases like cancer, has spurred intensive interest. Here, we report a robust stable isotope-diluted UHPLC–ESI-MS/MS method for accurate quantification of 12 purine ribonucleosides, including 10 methylated purine nucleosides. By the use of thermally decomposable ammonium bicarbonate (NH4HCO3) as a mobile phase additive for UHPLC–MS/MS detection, the ESI-MS/MS signal responses of these target compounds were enhanced by 1.7–24.5 folds. Noteworthily, three methylated guanosine isomers (m1G, m2G, and m7G) and two methylated adenosine isomers (m1A and m6A) that are indistinguishable directly by mass spectrometry were well resolved with optimal UHPLC separation. Combined with methanol extraction and solid-phase extraction (SPE) pretreatment, the method quantified intracellular concentrations of three modified nucleosides (Gm, m1G, and m2G), which would otherwise be undetectable because of significant suppression of their signals by the interfering cellular matrix. Nine purine nucleosides were simultaneously quantified in 293T cells, and their concentrations ranged by 4 orders of magnitude. Overall, the method presents high recovery rates over 90% for endogenous modified purine nucleosides in cultured cells, along with good precision, linearity, and LOD ranging from 0.30 fmol to 0.37 pmol per 5 × 105 cells. The developed UHPLC–MS/MS method holds potential for screening purine nucleosides as diagnostic and prognostic biomarkers and for quantifying purine epigenetic nucleosides post-cell metabolome analysis, thereby providing a valuable analytical tool for intracellular nucleoside quantification in future clinical research.
研究领域:
分析化学
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生物化学
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分子生物学
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癌症研究
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代谢组学
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DOI
PubMed
高影响因子
ANALYTICAL CHEMISTRY
·
2021
·
IF 6.986
Jinyi Wu,Shuyi Huang,Lei Tan,Yuling Li,Xiaotong Wu,Yong Liang
Dengue fever is caused by mosquito-transmitted dengue virus infection and continues to increase worldwide, threatening public health in tropical and subtropical regions. The primary difficulties in preventing a reduction of the medical burden of dengue fever lies in the lack of effective mosquito control, preventive dengue vaccines, and clinically effective antiviral drugs to treat dengue infections. Rapid and accurate diagnosis is crucial for proper patient care and effective control of epidemics. The present work proposes an alternative strategy for detecting the dengue virus nonstructural protein 1 (NS1) antigen in clinical serum samples by using ultrahigh-performance liquid chromatography tandem mass spectrometry (UHPLC–MS/MS) in combination with the molecularly imprinted polymers. Rather than the whole protein, the NS1 signature peptide is selected as a template for molecular imprinting and quantified as a stoichiometric readout of NS1. Three functional monomers with hydrophobic, positively charged, and negatively charged groups were synthesized by click reactions in terms of the signature peptide. These three functional monomers provide abundant recognition sites for the peptide, allowing the peptide template to be effectively imprinted during polymerization. The imprinting conditions were optimized, and the molecularly imprinted polymers were characterized and used for enriching the signature peptide from digested serum samples by solid-phase extraction and then detected by UHPLC–MS/MS. The proposed method is used to detect the dengue virus NS1 in clinical samples and holds significant promise for early confirmation of dengue virus infection.
研究领域:
医学诊断
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病毒学
·
分析化学
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DOI
高影响因子
Heliyon
·
2024
·
IF 3.4
Shunqin Chen,Han Yang,Shan Zhang,Faze Zhu,Shan Liu,Huan Gao,Qing Diao,Wenbo Ding,Yuemeng Chen,Peng Luo,Yubo Liu
This study developed an online solid-phase extraction ultra-high performance liquid chromatography-tandem mass spectrometry (Online-SPE-UHPLC-MS/MS) method for the analysis of 28 illegal drugs in sewage. To achieve this, 28 isotope internal standards (ISTDs) were added to 3 mL sewage samples, the pH was adjusted to 7–8 using hydrochloric acid or 20% ammonia water, followed by centrifugation, filtration, and analysis using UHPLC-MS/MS. The results indicated an excellent linearity of 1–300 ng L −1 , and cotinine in the concentration range of 20–6000 ng L −1 , linear correlation coefficient R 2 > 0.995, with the limit of detection (LOD) of 0.01–6 ng L −1 , and a limit of quantification (LOQ) of 0.1–20 ng L −1 . The addition of three concentrates of low (2 ng L −1 /40 ng L −1 ), medium (20 ng L −1 /400 ng L −1 ), and high concentration (200 ng L −1 /4000 ng L −1 ) demonstrated the matrix effect of the target compound between ± 22.0%. The extraction recovery was 70.0–119.4%, and a percent accuracy of 75.7–118.1%. Similarly, the intra- and inter-day precisions were 1.8–20.0% and 1.5–18.9%, respectively. The results cemented the sensitivity, accuracy, reliability, strong specificity, and reproducibility, which can be used to screen 28 illegal drugs in sewage for trace analysis.
研究领域:
环境科学
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分析化学
·
毒理学
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产品关联
DOI
PubMed
高影响因子
Journal of Natural Medicines
·
2026
·
IF 2.6
Mao Qiang,Zhong Huan,Liang Wan-Li,Dai Jin,Huang Rui-Ting,Wang Yi-Di,Sun Di-Yang,Tang Kai,Xia Long-Fei,Gong Hai-Biao,Li Yi-Fang,Sun Wan-Yang,Zhang Qiong-Yi,Zeng Li,Yu Li-Li,Xu You-Hua,Wu Qi-Biao,Zhu Yi-Zhun,Tan Hong-Li,Ouyang Shu-Hua,He Rong-Rong
Natural Calculus Bovis (NCB) and Bovis Calculus Sativus (BCS) are both used clinically but exhibit different therapeutic effects, the material basis of which remains unclear. Lipid-soluble components are hypothesized to contribute to these differences, however the compositional variations at the lipid level have not been fully characterized. In this study, untargeted UHPLC-MS/MS lipidomics was employed to compare the lipid profiles of NCB and BCS. The results indicated that both samples contained fatty acyls, glycerolipids (GL), glycerophospholipids (GP), sphingolipids (SP), and sterol lipids (ST), indicating a conserved core lipid framework. However, NCB showed higher lipid complexity and abundance. NCB contained higher levels and greater molecular diversity of intact GP (phosphatidylcholines and phosphatidylethanolamines), SP (ceramides), fatty acid-derived lipids (polyunsaturated N -acylethanolamines, PU-NAE), and sterol esters. In comparison, BCS exhibited a simplified profile dominated by GL, with reduced GP, SP and ST species, enrichment of lysophospholipids and bile acid-related sterols, and lower overall lipid abundance. These differences may result from distinct formation processes: prolonged in vivo maturation for NCB versus time-limited in vitro culturing for BCS. This study expands the current understanding of the material basis of NCB and BCS, from a lipidomic perspective, offering molecular insights into its pharmacological properties and providing a scientific foundation for the material basis, quality control, standardization and rational clinical application of Calculus Bovis . Graphical abstract The alternative text for this image may have been generated using AI.
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DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2025
·
IF 2.8
Yingxia Guo,Meichen Liu,Jiye Tian,Chunpeng Feng,Qingbin Wang,Xuan Zhao,Lei Yin
As an important chemical reagent, methoxy polyethylene glycol amine (mPEG-NH 2 ) is widely used in biomedical field. Unraveling the pharmacokinetic behavior of mPEG-NH 2 polymers is essential for revealing the toxicity and efficiency of mPEG-NH 2 related drug delivery systems. In this study, a simple analytical assay based on mass spectrometry (MS) was first established and validated for quantification of mPEG 5 -NH 2 in biological matrix. The multiple reaction monitoring (MRM) transitions at m / z 252.2 (precursor ions) → 87.7 (fragment ions) and m / z 371.2 (precursor ions) → 89.2 (fragment ions) were chosen to determine mPEG 5 -NH 2 and OH-PEG 8 -OH, respectively. The UHPLC-MS/MS assay showed excellent linearity over the range of 0.01–10 μg/mL. Intra-day and inter-day accuracies and precisions of the assay were all within ± 6.44 %. The analytical assay was successfully applied to reveal the in vivo pharmacokinetic behavior of mPEG 5 -NH 2 in rats.
研究领域:
药理学
·
分析化学
·
生物医学工程
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产品关联
DOI
PubMed
高影响因子
DRUG METABOLISM AND DISPOSITION
·
2026
·
IF 4
Jiye Tian,Jiarui Zhang,Zihan Tang,Chunpeng Feng,Yue Deng,Jiale Liu,Shuang Feng,Xinyue Zhou,Lei Yin,Meiyun Shi
A comprehensive understanding of the in vivo fate of low-molecular-weight polyethylene glycol (PEG) oligomers is essential for optimizing PEGylated therapeutics. This study delineates the polymerization-dependent absorption, distribution, metabolism, and excretion (ADME) of discrete PEG600 oligomers (n = 9–18) in rats using a validated UHPLC-MS/MS method. Systemic exposure, assessed by dose-normalized AUC, was highest for shorter oligomers (n = 9–10) and declined for longer chains (n ≥ 17), while all oligomers exhibited similarly short terminal half-lives (12.7–15.2 min), indicating rapid elimination irrespective of chain length. Tissue distribution revealed pronounced renal accumulation, peaking at mid-chain lengths (n = 11–13), consistent with size-dependent glomerular filtration and tubular reabsorption. Oxidative metabolism yielded both mono- and di-carboxylated derivatives, confirming active enzymatic processing. Excretion studies demonstrated chain-length-dependent elimination, with reduced recovery of longer oligomers suggesting substantial in vivo biodegradation. These findings provide the first monomer-resolved ADME profile of PEG600 oligomers, highlighting the critical role of polymerization degree in governing their pharmacokinetics and informing the rational design of PEGylated drug formulations.
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DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2026
·
IF 3.1
Xiaoyan Zhang,Shuang Feng,Ziluo Zhang,Chuya Wang,Yongshan Ai,Yalin Xi,Lei Yin,Meiyun Shi
This study established a robust and selective ultra-high-performance liquid chromatography–tandem mass spectrometry (UHPLC-MS/MS) method to investigate the excretion behavior of polyethylene glycol 1000 (PEG1K) oligomers (N = 13–26) in rats. PEG is widely used in pharmaceutical applications, particularly in drug delivery systems, yet detailed excretion profiles of lower molecular weight PEGs remain insufficiently characterized. The developed method utilized ammonium adducts ([M+NH₄]⁺) as precursor ions in multiple reaction monitoring mode, enabling sensitive and high-throughput quantification of individual oligomers in biological matrices. Following intravenous administration in rats, excretion kinetics were monitored over 48 hours. Cumulative recovery analysis revealed that renal excretion was the dominant elimination pathway, accounting for 47.30–68.52% of the administered dose in urine, while fecal excretion represented only 0.66–3.38%. These findings provide critical insights into the in vivo disposition of PEG1K, supporting its safety evaluation and rational application in drug formulation. The presented analytical platform offers a reliable tool for polymer pharmacokinetic studies.
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DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2026
·
IF 2.8
Haiyang Cui,Dongliang Yang,Yonggang Zheng,Jing Li,Hairui Yan,Xiaoli Gao
Steroids and their metabolites play crucial roles in reproductive health, endocrine diseases, and tumor development. Comprehensive analysis of these compounds is essential for both mechanistic investigations and clinical evaluations. Although comprehensive analytical methods have been established for steroids in human clinical samples, their direct application to rat specimens remains limited, particularly with the absence of validated methods for detecting certain hydroxylated steroid metabolites in vivo. This study developed highly sensitive solid-phase extraction coupled with ultra-high-performance liquid chromatography-tandem mass spectrometry methods for the quantitative analysis of 29 steroid metabolites. Through optimized derivatization of steroids and integration of two-dimensional liquid chromatography techniques, the method effectively reduces interference from non-volatile salts and overcomes trace-level detection challenges. Method validation demonstrated a wide linear range (0.002–250 ng/mL), low limits of quantification (2–100 pg/mL), high accuracy (88–114%), and precision (intra- and inter-batch CV ≤14%). The method exhibited acceptable extraction recovery, matrix effects, and stability, confirming compliance with regulatory standards. The validated method was successfully applied to characterize serum steroid metabolic profiles in both N -methyl-N-nitrosourea-induced breast cancer and ovariectomized rat models, revealing alterations in estrogen 2-hydroxylation and pregnenolone 21-hydroxylation pathways mediated by key steroidogenic enzymes, including CYP1A1/CYP1B1 and potentially CYP21A2-independent mechanisms, providing robust support for preclinical research on steroid-related diseases.
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产品关联
DOI
PubMed
高影响因子
危险品化学品经营许可证（带存储）