JOURNAL OF SEPARATION SCIENCE
·
2025
·Vol. 48
·期 8
·e70253
·
IF 2.8
Difeng Zhu,Jing Dou,Li Ping,Yawen Hong,Chao Chen,Chenxing Yuan,Qixiu Li,Wenjie Luo,Xiaoqing Chi
Aerosol inhalation therapy offers significant benefits in treating chronic obstructive pulmonary disease, including rapid onset of action and reduced systemic side effects. Revefenacin, a long-acting bronchodilator, has demonstrated efficacy in improving lung function and alleviating chronic obstructive pulmonary disease symptoms through aerosol delivery. However, quantitative methods for determining the inhaled concentration of revefenacin aerosol remain limited. This study developed and validated a rapid, robust ultrahigh-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method to quantify revefenacin aerosol concentration. The method, with an analysis time of 2 min, exhibited excellent specificity, precision, and a lower limit of quantification of 2 ng/mL. The aerosol extraction recovery averaged 98.5%. The method was successfully applied to assess aerosol concentration and aerodynamic particle size distribution under different sampling conditions. Results showed that after 15 min of nebulization, the average aerosol concentrations collected using syringe aspiration and impactor sampling methods were 0.98 and 0.95 mg/m 3 , respectively, demonstrating consistency between the techniques. Aerodynamic particle size distribution analysis revealed stable particle size distribution with atomization times of 5 and 15 min, yielding mass median aerodynamic diameters of 2.31 and 2.35 µm, fine particle fractions of 76.5% and 76.7%, and geometric standard deviations of 2.44 and 2.41, respectively. These findings indicate that the aerodynamic properties of revefenacin aerosol remain stable over prolonged nebulization. This study establishes a reliable analytical method for revefenacin aerosol quantification and provides valuable insights into its aerodynamic characteristics, supporting its further application in chronic obstructive pulmonary disease treatment.
研究领域:
药物分析
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肺部给药
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分析化学
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呼吸系统疾病
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DOI
PubMed
高影响因子
LWT-FOOD SCIENCE AND TECHNOLOGY
·
2021
·
IF 4.952
Lingrong Wen,Mingyang He,Chunxiao Yin,Yueming Jiang,Donghui Luo,Bao Yang
Sour orange ( Citrus aurantium ) is a popular fruit with health benefits. Phenolics are the dominant bioactive compounds in this fruit. However, the full phenolics composition remains unclear. In this work, UHPLC-MS/MS was used to qualify and quantify the phenolics in sour orange fruits of cv. Morocco (MSO) and United (USO). Fifty-eight phenolics, including 26 flavonoid glycosides , 22 polymethoxylated flavonoids, 8 coumarins and 2 phenolic acids , were identified. Four limonoids were characterized. Flavonoid glycosides were the leading phenolics in MSO, while polymethoxylated flavonoids (including nobiletin, tangeritin and sinensetin) were dominant in USO. The phenolic extracts showed good antioxidant activities . USO extract had a significantly ( p < 0.05) stronger neuroprotective activity than MSO extract. Auraptene, nobiletin and tangeritin were highly responsible for the neuroprotective activity. The results were helpful for the development of functional foods with sour orange.
研究领域:
食品科学
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药理学
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分析化学
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产品关联
DOI
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2022
·
IF 4.601
Hongyu Ning,Yilei Fan,Huijun Liu,Zhongping Huang,Xing Ke,Yu Xu,Yuanbin She
A novel mixed-mode weak cation-exchange sorbent (PS-DVB-WCX-II) was prepared by the modification of polystyrene-divinylbenzene with mercaptosuccinic acid for the selective extraction of illicit drugs in environmental water. The PS-DVB-WCX-II was synthesized through the Friedel-Crafts acylation reaction on the surface of polystyrene-divinylbenzene, followed by nucleophilic substitution reaction and thiol-ene click reaction. The sorbent can selectively absorb illicit drugs through the reverse-phase interactions provided by benzene ring on the polymer backbone and the ion-exchange interactions provided by functional group (-COOH). As compared with the extraction performance of three commercial SPE cartridges, it was found that the prepared sorbent had better adsorption performance with the recovery values between 84.1% and 106.0% for the selected 11 illicit drugs under the optimized SPE conditions. Illicit drugs in environmental water were extracted by the sorbent, prior to the detection of UHPLC-MS/MS. Two quantitative methods were established respectively for the detection of 11 illicit drugs in different matrices of river water and wastewater. Both methods had good determination coefficient (r 2 >0.992) in the range of 0.5–50 ng/L, 2.5–250 ng/L, 5–500 ng/L, and low limits of detection ( S / N = 3) of 0.17–1.67 ng/L. In the real wastewater samples, the concentration of morphine was 18.3–126.3 ng/L, and the methamphetamine was 12.7–27.4 ng/L. Meanwhile, PS-DVB-WCX-II was compared with Oasis MCX and Oasis HLB in the detection of real wastewater samples. The results revealed that PS-DVB-WCX-II and Oasis MCX had better performance in absorbing methamphetamine than Oasis HLB, and PS-DVB-WCX-II had better ability to remove the matrix. The results suggested that the prepared weak cation-exchange sorbent had the potential in the application of illicit drug detection in environmental water.
研究领域:
分析化学
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环境科学
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产品关联
DOI
PubMed
高影响因子
Foods
·
2026
·Vol. 15
·期 16
·2855
·
IF 6
Haijie Huang,Li Zhao,Zhikai Wang,Yang Qiao,Huidong Deng,Yingjun Ye,Kaili Ding,Xuejie Feng,Yijun Liu
To investigate the differences in pulp metabolites among four varieties of Pouteria caimito fruit (JZL1, JZL3, JZL5, and JZL6), ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) was employed for the separation and identification of metabolites. A total of 1285 metabolites were identified, including 648 in positive ion mode and 637 in negative ion mode. At the class level, carboxylic acids and derivatives (14.32%) and organooxygen compounds (11.83%) accounted for the highest proportions; at the subclass level, amino acids, peptides, and analogues (12.53%) as well as carbohydrates and carbohydrate conjugates (9.49%) were the main categories. PLS-DA analysis revealed significant differences in metabolite profiles among the four varieties, with numerous up-regulated and down-regulated metabolites in each comparison group, and some metabolites showed fold changes > 10 or <0.1. KEGG pathway enrichment analysis further indicated that differential metabolites were primarily enriched in pathways such as ABC transporters, citrate cycle (TCA cycle), starch and sucrose metabolism, and linoleic acid metabolism. This study provides an important metabolomic basis for variety identification, nutritional quality evaluation, and functional component development of Pouteria caimito fruit.
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产品关联
DOI
PubMed
高影响因子
Separation Science Plus
·
2025
·Vol. 8
·期 6
·e70069
·
IF 1.6
Yilin Li,Li Song,Yan Liang,Hui Li
QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) is a pretreatment technique based on dispersive solid-phase extraction. This study employs QuEChERS technology in preprocessing plasma samples, combined with high-performance mass spectrometry, to quantify the concentrations of six drugs (used in the treatment of cardiovascular and cerebrovascular diseases: butylphthalide, clopidogrel, rosuvastatin, ramipril, atenolol, and simvastatin). This method utilizes 3 mL of acetonitrile as a precipitant, 500 mg of anhydrous magnesium sulfate as a salt precipitation agent, and 10 mg of C18 as an adsorbent for treating plasma samples. Chromatographic separation was carried out using a Shim-pack GIST C18 from Shimadzu (2.1 × 100 mm; 2 µm), with a mobile phase consisting of 0.1% methanol and 0.1% water, detected in ESI positive ion mode. N -butylphthalide, clopidogrel, and rosuvastatin demonstrated linear relationships within the range of 1–100 ng/mL, while ramipril and atenolol exhibited linear relationships within the range of 2–200 ng/mL. Simvastatin exhibited linear relationships in the range of 4–400 ng/mL. All linear equations exhibit R 2 values exceeding 0.990, and the methodological validation results meet the requirements. The method offers the advantages of rapidity, simplicity of operation, and high accuracy, making it suitable for drug detection in patients with hypertension, hyperlipidemia, or stroke.
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产品关联
DOI
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2016
·
IF 2.687
Pengfei Zhu,Xia Ling,Wenwei Liu,Lingcan Kong,Yuyang Yao
A simple and fast analytical method for determination of eleven Polyfluorinated Compounds (PFCs) in source water was developed in the present work. The water sample was prepared without filtered through microfiltration membrane and 500 mL of source water was enriched by the solid phase extraction (SPE). The targent compounds were analyzed by ultra high performance liquid chromatography–tandem mass spectrometry (UHPLC–MS/MS). The optimized analytical method was validated in terms of recovery, precision and method detection limits (MDLs). The recovery values after correction with the corresponding labeled standard were between 97.3 and 113.0% for samples spiked at 5 ng/L, 10 ng/L and 20 ng/L. All PFCs showed good linearity and the linear correlation coefficient was over 0.99. The precisions were 1.0–9.0% (n = 6). As the result of the enrichment, the MDL values ranged from 0.03 to 1.9 ng/L and were enough for analysis of the trace levels of PFCs in the Taihu Lake. The method was further validated in determining the source water and the results showed that PFHxS, PFHxA, PFOA and PFOS were the primary PFCs in Taihu Lake which might be different from the other researches. The method can be used for determination of PFCs in water with a stable recovery, good reproducibility, low detection limit, less solvent consumption, time saving and labor saving. To our knowledge, this is the first method that describes the effect of the filter membrane on the determination of PFCs in water which might acquire more accurate concentration of PFCs in Taihu Lake.
研究领域:
环境科学
·
分析化学
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产品关联
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
·
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
·
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
BIOMEDICAL CHROMATOGRAPHY
·
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
·
毒理学
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产品关联
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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产品关联
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
·
病毒学
·
分析化学
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DOI
高影响因子
危险品化学品经营许可证（带存储）