MOLECULES
·
2024
·Vol. 29
·期 5
·1055
·
IF 4.2
Jing Xu,Xiu-Wei Yang
Berberine is a natural isoquinoline alkaloid with low toxicity, which exists in a wide variety of medicinal plants. Berberine has been demonstrated to exhibit potent prevention of indomethacin-induced gastric injury (GI) but the related mechanism remains unclear. In the present study, liquid chromatography-mass spectrometry (LC-MS)-based metabolomics was applied for the first time to investigate the alteration of serum metabolites in the protection of berberine against indomethacin-induced gastric injury in rats. Subsequently, bioinformatics was utilized to analyze the potential metabolic pathway of the anti-GI effect of berberine. The pharmacodynamic data indicated that berberine could ameliorate gastric pathological damage, inhibit the level of proinflammatory factors in serum, and increase the level of antioxidant factors in serum. The LC-MS-based metabolomics analysis conducted in this study demonstrated the presence of 57 differential metabolites in the serum of rats with induced GI caused by indomethacin, which was associated with 29 metabolic pathways. Moreover, the study revealed that berberine showed a significant impact on the differential metabolites, with 45 differential metabolites being reported between the model group and the group treated with berberine. The differential metabolites were associated with 24 metabolic pathways, and berberine administration regulated 14 of the 57 differential metabolites, affecting 14 of the 29 metabolic pathways. The primary metabolic pathways affected were glutathione metabolism and arachidonic acid metabolism. Based on the results, it can be concluded that berberine has a gastroprotective effect on the GI. This study is particularly significant since it is the first to elucidate the mechanism of berberine’s action on GI. The results suggest that berberine’s action may be related to energy metabolism, oxidative stress, and inflammation regulation. These findings may pave the way for the development of new therapeutic interventions for the prevention and management of NSAID-induced GI disorders.
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PubMed
高影响因子
Food Analytical Methods
·
2016
·Vol. 10
·期 5
·1386-1396
·
IF 2.167
Wang Yu,Gao Lei,Qin Dongli,Chen Ligang
In this work, a simple and selective method based on matrix solid phase dispersion (MSPD) using molecularly imprinted polymers (MIPs) as sorbents was successfully developed for the determination of melamine (MEL) in milk powder. The MIPs have been prepared by surface imprinted polymerization method using carbon nanotube (CNT) as support, MEL as template molecule, γ-aminopropyltriethoxysilane as functional monomer, and tetraethyl orthosilicate as cross-linking agent. The MIPs were characterized by Fourier transform infrared spectrometer and scanning electron microscopy. At the same time, the adsorption isotherm, dynamic adsorption, and selective adsorption of MIPs to MEL were also studied. The prepared MIPs were used as dispersant of MSPD to extraction and separate MEL in milk powder. We optimized the extraction conditions as follows: the ratio of MIPs to sample was 2:3; the dispersion time was 10 min; washing solvent was 2.0 mL acetonitrile; and elution solvent was 4.0 mL ammonium methanol (5:95, v / v ). Once the MSPD process was completed, the MEL extracted from milk powder was determined by LC-MS/MS. Under the optimal conditions, the limit of detection of MEL was 0.2 ng g −1 . The relative standard deviations of intra-day and inter-day were obtained in the range of 0.4∼5.1 %. The satisfied recoveries of MEL were 92.5∼97.2 %. The MIP-MSPD method has some advantages, such as higher selectivity, lower cost of preparation, less time consuming and organic solvent consumption, simpler sample pretreatment procedure, and higher extraction recovery compared with those existing methods which were used for determination of MEL.
研究领域:
食品科学
·
分析化学
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DOI
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2017
·
IF 2.603
Lingli He,Chuan Li,Xuyuan Liu,Qingqing Yang,Haizhi Zhang,Weiren Xu,Luyong Zhang,Changxiao Liu
Benzbromarone is a uricosuric drug metabolized predominantly by cytochrome P450 2C9 from in vitro findings. Human CYP2C9 exhibits extensive genetic polymorphism and numbers of clinic studies have demonstrated that CYP2C9 genetic polymorphism has a significant influence on the pharmacokinetics of benzbromarone. But in vitro study on the interaction between CYP2C9 allelic isoforms and benzbromarone was rare. Here, an LC–MS/MS method was established and validated to determine the concentration of benzbromarone in different CYP2C9 enzyme incubation systems for the drug-enzyme interaction study. By selecting appropriate internal standard and optimizing separation system, including mobile phase , sample solvent and gradient elution condition, this LC–MS/MS method was developed with fine linearity (r 2 ≥ 0.996), good reproducibility (RSD ≤ 6.6%), high stability (92.37–114.67%), efficient recovery (91.23–109.82%) and acceptable matrix effect (110.54–115.31%). Based on this method, the interaction between 3 CYP2C9 allelic isoforms and benzbromarone was researched by kinetics parameters (K m , V max , Cl int ). As a result, CYP2C9*1 displayed the highest metabolic activity towards benzbromarone, CYP2C9*2 showed a little lower catalytic activity than CYP2C9*1 (relative clearance/*1 = 85.86%), CYP2C9*3 showed the lowest catalytic activity (relative clearance/*1 = 21.57%). The result illustrated that various CYP2C9 allelic isoforms showed different enzymatic activities towards benzbromarone, which could offer effective consultation for personalized administration in clinic.
研究领域:
药理学
·
医学遗传学
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DOI
PubMed
高影响因子
Food Quality and Safety
·
2022
·
IF 3.949
Kang Yuting,Li Chenghua,Li Huiru,Li Jing,Jiang Kezhi
Polycarboxylic acids (PACs) are important metabolic products in almost all living bodies, yet current analytical methods for detection of PACs in tea beverages are still unsatisfactory due to the complex matrix and physicochemical properties of PACs. In this work, a rapid method was developed for the simultaneous determination of 7 PACs, including tartaric acid, α-ketoglutaric acid, malic acid, malonic acid, cis-aconitic acid, succinic acid, and fumaric acid, in beverages, based on selective removal of the matrix in combination with liquid chromatography–mass spectrometry (LC-MS) analysis. By stirring with activated carbon and the Na2CO3 solution, the matrix in beverages was selectively removed, and PACs were almost retained in the supernatant of diluted Na2CO3 solution. Under optimized parameters, the limit of quantitation for the PACs was in the range of 1–50 ng/mL, and the content of the PACs in 8 beverages was determined with the recovery range of 72.2%–122.5%. The contents of malic acid, malonic acid, and succinic acid in tea beverages were found to be greater than those in non-tea beverages. Moreover, the concentration of these PACs in beverages was found to be multiplied many times in their deterioration period, especially for fumaric acid and α-ketoglutaric acid. These results indicated that PACs can be selected as a criterion to differentiate qualified tea beverages from spoiled beverages.
研究领域:
食品科学
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分析化学
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DOI
高影响因子
RAPID COMMUNICATIONS IN MASS SPECTROMETRY
·
2022
·Vol. 37
·期 1
·e9397
·
IF 2.586
Wenrui Yao,Jinfeng Ge,Qiaozhuan Hu,Jingying Ma,Daohe Yuan,Xiaoli Fu,Yulin Qi,Dietrich A. Volmer
Rationale The development of appropriate analytical screening techniques for pharmaceuticals and personal care products (PPCPs) is the basis for studying the distribution and environmental impact of emerging contaminants (ECs). Mass spectrometry-based screening methods vary with the complexity of the target compounds. It is challenging to balance both positive and negative ion quantification with a low detection limit. To establish a set of experimental methods including extraction, chromatography-separation and mass spectrometry screening is one of the most important topics in PPCP research. This paper describes a universal and efficient qualification and quantification protocol for the simultaneous detection of 34 PPCPs in different environmental samples in a single analytical data acquisition run. Methods Thirty-four representative PPCPs, which are widely distributed in the environment with high ecological toxicity and complex chemical structures, were selected as representative target ECs. The extraction of the target PPCPs was achieved using only one solid-phase extraction cartridge without the need to adjust the pH of samples. The enriched samples were detected by LC–MS/MS in both positive and negative ion modes simultaneously. The protocol was evaluated based on the accuracy, precision, detection limits and matrix effects. Results This method achieved simultaneous detection of PPCPs in both positive and negative ion modes, with a single analytical cycle of 12 min. The observed SPE recoveries were between 40% and 115%. The instrumental detection limits (IDL) varied from 0.01 to 1 pg, and the method detection limits (MDL) were between 0.002 and 3.323 ng/l in different matrices. Most of the PPCPs were subjected to matrix suppression below 30%. The method was successfully applied for quantitative analysis of the PPCPs in different environmental samples, including river samples, wastewater treatment plant (WWTP) samples and soil samples. Conclusions This protocol developed a rapid and efficient detection method to simultaneous qualitative and quantitative 34 representative PPCPs in the environment. The IDL ranged from 0.01 to 1 pg and the MDL ranged from 0.002 to 3.323 ng/l in different matrices. The detection limit was one order of magnitude lower compared to previous studies. The protocol also provided a wide application range for different environmental matrices, which permitted the migration and transformation of PPCPs to be explored.
研究领域:
环境科学
·
分析化学
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PubMed
高影响因子
Separations
·
2023
·Vol. 10
·期 9
·515
·
IF 2.6
Xiaodong Wang,Wenhao Wang,Qinggui Lei,Zhengming Qian,Wenbin Deng
This study aims to develop a fast and eco-friendly liquid chromatography–mass spectrometry (LC-MS) method for the determination of aesculin and aesculetin in Cortex Fraxini. Ultrapure water was used as the solvent during the microwave-assisted extraction process to prepare the Cortex Fraxini sample. This extraction method reduces the cost of the harmful solvent (only ultrapure water was used) and microwave extraction time (1 min). The LC separation was conducted using an Agilent InfinityLab Poroshell 120 EC-C18column (2.1 mm × 30 mm, 2.7 µm) with a mobile phase consisting of 0.1% formic acid and acetonitrile (90:10,v/v) at a flow rate of 0.6 mL/min. Isocratic elution was employed, and the analytes were detected by MS. Through careful optimization and selection of LC-MS conditions, the analysis time was reduced to 1 min, demonstrating the method’s efficiency. The developed method was validated and exhibited excellent specificity, linearity, limit, precision, accuracy, and stability in quantifying aesculin and aesculetin in the Cortex Fraxini samples. The analysis result revealed the presence of aesculin (ranging from 3.55 to 18.8 mg/g) and aesculetin (ranging from 1.01 to 16.2 mg/g) in all ten batches of Cortex Fraxini samples. Compared to the reported LC methods, this approach substantially reduces the total analysis time and requires a minuscule volume of organic solvents. An “Analytical Eco-Scale” assessment was used to evaluate the different assay methods of Cortex Fraxini. The current LC-MS method scored an impressive 90; it was better than the other four reports’ LC methods. Thus, the developed LC-MS method is rapid and green, which is helpful for the quality evaluation of Cortex Fraxini.Keywords:LC-MS;Cortex Fraxini;aesculin;aesculetin;green;fast
研究领域:
药学
·
分析化学
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DOI
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2022
·
IF 4.601
Jialing Huang,Yunqing Qi,Xiaowen Zeng,Wei Huang,Da Chen
Measurement of immunoglobulin subclasses is a useful tool for exploring humoral immune deficiency in the presence of total immunoglobulins within reference intervals. Conventional methods for immunoglobulin measurement are mostly immunoassays, which are of low throughput and laborious to run multiple immunoglobulin subclass tests. Liquid chromatography-mass spectrometry (LC-MS) has emerged as a promising technology for the measurement of protein biomarkers in biological matrices, owing to its high specificity, selectivity, multiplexing, and wide dynamic range. In fully taking these advantages, we developed here a LC-MS based methodology for simultaneous quantitation of the primary immunoglobulin isotypes (IgG, IgA, IgM) and their subclasses in human plasma. Method validation demonstrated that the proposed method showed good linearity with R > 0.99, high precision with coefficients of variation for inter- and intra-assay less than 15%, as well as high accuracy with relative errors less than 8.7%. The developed method was further applied to maternal and cord blood collected at delivery for assessment of maternal and fetal immune status. The immunoglobulin profiles and the features of transplacental transport of maternal immunoglobulin subclasses were comparable to the findings from previous reports, further demonstrating the reliability of this method. Therefore, our method provides a competitive approach to high-throughput detection of multiple immunoglobulin subclasses for biomonitoring or epidemiological studies.
研究领域:
免疫学
·
临床化学
·
妊娠研究
·
蛋白质组学
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PubMed
高影响因子
Scientific Reports
·
2025
·Vol. 15
·期 1
·1-8
·
IF 3.9
Liu Hao,Cai Meng,Peng Yong,Miao Jing-kun,Yu Jin
While remifentanil, etomidate, and rocuronium are increasingly used for cesarean section due to their favorable hemodynamic stability and fetal safety profile, their pharmacokinetics and potential effects on neonates remain poorly understood. This study developed and validated a rapid, sensitive LC–MS/MS method for simultaneous quantification of the three anesthetics in microsamples of 10 μl serum, followed by a paired maternal and umbilical cord serum investigation. After protein precipitation with acetonitrile, analytes were separated within 4 min using positive electrospray ionization in MRM mode. Method validation demonstrated excellent linearity (R 2 > 0.99) for all compounds, with LLOQs of 0.15 ± 0.02 ng/mL (remifentanil), 16.87 ± 0.51 ng/mL (etomidate), and 106.73 ± 8.63 ng/mL (rocuronium). Precision (intra-/inter-day < 15%) and minimal carry-over (< 5%) met bioanalytical standards. Applied to 20 maternal-newborn pairs, the method quantified differential drug distribution: maternal arterial concentrations (remifentanil 4.75 ± 0.19 ng/mL; etomidate 412.71 ± 35.29 ng/mL; rocuronium 7.08 ± 0.48 μg/mL) exceeded umbilical vein levels (2.43 ± 0.13 ng/mL; 302.15 ± 29.03 ng/mL; 0.86 ± 0.16 μg/mL), which were higher than umbilical artery concentrations (1.33 ± 0.15 ng/mL; 166.24 ± 21.53 ng/mL; 0.44 ± 0.77 μg/mL). Calculated placental transfer rates significantly differed among anesthetics (remifentanil 0.52 ± 0.02; etomidate 0.75 ± 0.04; rocuronium 0.13 ± 0.02; all P < 0.001), reflecting distinct pharmacokinetic behaviors. The validated method enables reliable microvolume analysis for perinatal pharmacokinetic studies, particularly valuable when sample availability is limited. Its rapid throughput and sensitivity make it suitable for clinical research applications investigating maternal–fetal drug transfer dynamics.
研究领域:
分析化学
·
药代动力学
·
麻醉学
·
妇产科学
·
新生儿学
·
临床研究
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DOI
PubMed
高影响因子
TALANTA
·
2024
·
IF 5.6
Jie Han,Qinyan Yang,Zheng Zhi,Na Li,Jian-Lin Wu
Carboxyl: or carbonyl-containing metabolites (CoCCMs) are widely distributed in biological samples. Global profiling of CoCCMs is essential for ascertaining specific functions of metabolites and their potential physiological roles in biogenic activities. However, simultaneous determination of these compounds is hampered by poor ionization efficiency, vast polarity differences, wide discrepancy of concentration ranges. Herein, a novel bromine isotope derivatization reagent 5-bromo-2- hydrazinopyridine was employed for CoCCMs profiling by liquid chromatography-mass spectrometry (LC-MS). This method enabled rapid derivatization of 44 CoCCMs under mild conditions. Enhanced separation efficiencies, detection sensitivities, and distinctive MS fragmentation characteristics were observed. Furthermore, this method was demonstrated to be efficient in revealing metabolic alternations, and abnormal serum levels of 6-keto-PGF1α, 12(S)-HHTrE, 15(S)-HEPE and N -acetyl tryptophan were disclosed for the first time in Mycoplasma pneumoniae (MP) infectious patients. Finally, based on the distinctive 2 Da differences of molecular ion peak pairs with almost 1:1 intensity ratio originated from 79 Br and 81 Br isotopes, an MS-DIAL and Python assisted MS1 isotope screening-MS2 fragments characterization combination strategy was developed for rapid screening, classification, and identification of detected CoCCMs. A total of 1,069 CoCCMs were detected, of which 198 CoCCMs were identified in untargeted analysis. Statistical analysis revealed altered metabolic pathways, while glutamic acid, oxoglutaric acid, succinic acid, pyruvic acid, glyceric acid, and glycine were selected as potential biomarkers of MP infection. This bromine signature coded derivatization-LC-MS approach was proved to be a valuable tool for global probing of CoCCMs in biological samples with high sensitivity and broad coverage.
研究领域:
医学
·
生物化学
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DOI
PubMed
高影响因子
Scientific Reports
·
2020
·Vol. 10
·期 1
·1-11
·
IF 3.998
Zhou You,Qin De Qiang,Zhang Pei Wen,Chen Xiao Tian,Liu Ben Ju,Cheng Dong Mei,Zhang Zhi Xiang
Azadirachtin exhibits excellent bioactivities against several hundred arthropods. However, current knowlege of its biochemical effect on B . dorsalis larvae is not deep enough. In this study, integrated LC-MS and GC-MS-based untargeted metabolomics were used to analyze the changes of endogenous metabolites and the biochemical effects of azadirachtin on B . dorsalis larvae. Azadirachtin has excellent bioactivities against B . dorsalis larvae in this study, leading to a longer developmental duration, lower survival rate, and low pupa weight. The effect of azadirachtin was investigated on a total of 22 and 13 differentially abundant metabolites in the LC–MS and GC–MS-based metabolomics results, are selected respectively. Pathway analysis indicated that 14 differentially enriched metabolic pathways, including seven influential pathways, are worthy of attention. Further integrated key metabolic pathway analysis showed that histidine metabolism, d -glutamine and d -glutamate metabolism, biotin metabolism, ascorbate and aldarate metabolism, pentose and glucuronate interconversions, and alanine, aspartate and glutamate metabolism in B . dorsalis larvae are significantly relevant pathways affected by azadirachtin. Although extrapolating the bioactivity results in this study to the practical project of B . dorsalis pest management in the field has limitations, it was found that azadirachtin has a significant effect on the primary metabolism of B . dorsalis larvae.
研究领域:
昆虫学
·
代谢组学
·
植物化学
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DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2015
·
IF 2.979
Lei Liu,Na Cao,Xingling Ma,Kaihe Xiong,Lili Sun,Qiaogen Zou,Lili Yao
The current study reports the development and validation of a stability-indicating reversed phase HPLC method for the separation and identification of potential impurities in vortioxetine, a recently developed antidepressant. The structures of a new compound and four process-related impurities formed during the synthesis were characterized and confirmed by NMR, MS, and IR spectroscopy analyses. The most probable formation mechanisms of the impurities identified were proposed. Based on the characterization data, the new compound was proposed to be 1-[4-[(2,4-dimethylphenyl)thio]phenyl]-piperazine. In addition, an efficient chromatographic method was optimized to separate and quantify the impurities, which were obtained in the 0.05–0.75 μg/mL range. The developed HPLC method was validated with respect to accuracy, precision, linearity, robustness, and limits of detection and quantitation.
研究领域:
药物分析
·
分析化学
·
药学
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DOI
PubMed
高影响因子
Analytical Methods
·
2015
·Vol. 7
·期 12
·4919-4926
·
IF 1.821
Jun-Qing Zhang,Yong Wang,Hai-Long Li,Qi Wen,Hang Yin,Nian-Kai Zeng,Wei-Yong Lai,Na Wei,Shou-Qian Cheng,Sheng-Li Kang,Feng Chen,You-Bin Li
The rhizomes of Alpinia officinarum Hance (Zingiberaceae family) have been used as antiemetics, stomachics and analgesics in Asia for centuries. Unfortunately, the aerial parts were thrown away as waste whilst harvesting the rhizomes of A. officinarum. Recently, scientists reported that the ethanol extract of the aerial parts displayed anti-proliferation activity through mitochondrial pathway-induced cell apoptosis. However, the chemical composition of this extract remained largely unknown. We have identified sixteen chemicals including twelve flavonoids and four diarylheptanoids from the methanol extract of A. officinarum leaves using liquid chromatography/tandem mass spectrometry (LC-MS/MS). In order to better explore the potential value of the aerial parts, we need to know what the main constituents occurring in the aerial parts are and how the content of these chemicals is influenced by growing period. In the present study, a LC-MS/MS method was developed and validated for determination of seventeen compounds occurring both in the aerial parts and rhizomes sampled at different growing periods. The validation indices evaluated were satisfactory and the method was successfully employed to analyze the above-mentioned plant samples. Notably, we found that the content of these compounds, except for quercetin, was higher in rhizomes than in aerial parts. The six major constituents both in the aerial parts and rhizomes were galangin, kaempferide, hexahydrocurcumin, pinocembrin, chrysin and isorhamnetin. Moreover, the trends of change in content along with the sample period for most of the monitored phytochemicals were almost similar between the aerial parts and rhizomes. Our study should be of value in arousing everyone's interest to make the best use of the aerial parts of A. officinarum in the future.
研究领域:
药用植物学
·
分析化学
·
植物科学
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DOI
高影响因子
危险品化学品经营许可证（带存储）