JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2025
·
IF 3.1
Yu Qin,Shenping Zhang,Jingwen Shi,Heng Gong
Antibiotics are a class of compounds that are effective against bacterial infections and are widely used in aquaculture. Herein, a method based on high performance liquid chromatography coupled with tandem mass spectrometry was developed to detect nine classes of 116 antibiotics in aquatic products. The antibiotics were extracted in two steps using 1% formic acid-acetonitrile with 0.1 mol/L Na 2 EDTA-Mcllvain buffer solution and acetonitrile, purified using Captiva EMR-Lipid, and separated with an ACQUITY UPLC®HSS T 3 column (100 mm×2.1 mm, 3.5 μm) using acetonitrile and 0.1% formic acid with 5 mM ammonium acetate as mobile phase for gradient elution. Calibration curve from 0.10 to 100 ng/mL exhibited good correlation coefficient (R 2 >0.99) for quantification. The analytical performance of the developed method was satisfactory, with limits of quantification ≤ 5.00 ng/g for detecting of antibiotics in aquatic products. The recoveries of the 116 antibiotics ranged from 60.57% to 127.33%, with precision (expressed as relative standard deviation) of < 30.20%. All parameters showed acceptable values and conformed to the Commission Decision 2021/808/EC criteria. When compared with other techniques, the developed method meets the quantitative requirements of high-throughput analysis and can simultaneously analyze 116 antibiotics in aquatic products.
研究领域:
分析化学
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食品科学
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环境科学
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药理学
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DOI
PubMed
高影响因子
MICROCHIMICA ACTA
·
2018
·Vol. 185
·期 6
·1-10
·
IF 5.705
Yang Wen,Li Tengfei,Shu Chang,Ji Shunli,Wang Lei,Wang Yan,Li Duo,Mtalimanja Michael,Sun Luning,Ding Li
A method is described for the determination of proteins with LC-MS/MS enabled by a small molecule (adenosine) barcode and based on a double-recognition sandwich structure. The coagulation protein thrombin was chosen as the model analyte. Magnetic nanoparticles were functionalized with aptamer29 (MNP/apt29) and used to capture thrombin from the samples. MNP/apt29 forms a sandwich with functionalized gold nanoparticles modified with (a) aptamer15 acting as thrombin-recognizing element and (b) a large number of adenosine as mass barcodes. The sandwich formed (MNP/apt29-thrombin-apt15/AuNP/adenosine) can ben magnetically separated from the sample. Mass barcodes are subsequently released from the sandwiched structure for further analysis by adding 11-mercaptoundecanoic acid. Adenosine is then detected by LC-MS/MS as it reflects the level of thrombin with impressively amplified signal. Numerous adenosines introduced into the sandwich proportional to the target concentration further amplify the signal. Under optimized conditions, the response is linearly proportional to the thrombin concentration in the range of 0.02 nM to 10 nM, with a detection limit of 9 fM. The application of this method to the determination of thrombin in spiked plasma samples gave recoveries that ranged from 92.3% to 104.7%.
Schematic representation of a method for the determination of thrombin with LC-MS/MS. The method is based on a double-recognition sandwiched structure. With LC-MS/MS, mass barcodes (adenosine) are detected to quantify thrombin, which amplifies the detection signal impressively.
研究领域:
分析化学
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蛋白质组学
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医学检测
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PubMed
高影响因子
INTERNATIONAL JOURNAL OF LEGAL MEDICINE
·
2024
·Vol. 138
·期 4
·1323-1328
·
IF 2.2
Yu Zhonghao,Zhao Erjuan,Shi Qing,Yuan Yuhao,Ma Jinghong,Zhou Luwang,Duan Yijie,Zhou Yiwu
Brodifacoum exerts its antagonistic effect against the metabolism of vitamin K, an essential component in the synthesis of blood coagulation factors. This effect ultimately hinders the blood’s capacity to clot effectively, rendering it a commonly employed rodenticide. Instances of lethal poisonings are exceedingly rare owing to expeditious medical intervention and treatment. Within this report, we present a case of brodifacoum-induced homicide, wherein the patient exhibited distinct clinical examinations and symptoms. Moreover, the patient’s blood sample exhibited a noteworthy brodifacoum concentration of 0.681 µg/mL even after a period of 43 days following the incident of poisoning. Although an autopsy was not conducted due to religious restrictions, we endeavor to reasonably deduce the cause of death and furnish corroborative evidence for clinical diagnosis, treatment, and forensic examination in instances involving brodifacoum poisoning.
研究领域:
医学
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毒理学
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法医学
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DOI
PubMed
高影响因子
ENVIRONMENTAL SCIENCE AND POLLUTION RESEARCH
·
2016
·Vol. 23
·期 9
·8500-8507
·
IF 2.76
Wang Dezhen,Zhang Ping,Wang Xinru,Wang Yao,Zhou Zhiqiang,Zhu Wentao
In the present study, both untargeted and targeted metabolomics approaches were used to evaluate the subacute effects of hexabromocyclododecane (HBCD) on mice urine metabolome. Untargeted metabolomics based on 1 H NMR showed that HBCD exposure disturbed mice metabolism in both dosed groups, especially in high dosed group. The low-dose HBCD led to a decrease in alanine, malonic acid, and trimethylamine (TMA). High-dose HBCD-treated mice developed high levels of citric acid and 2-ketoglutarate, together with decreased alanine, acetate, formate, TMA, 3-hydroxybutyrate, and malonic acid. Targeted metabolomics for metabolic profiling of 20 amino acids identified alanine, lysine, and phenylalanine as significantly disturbed metabolites. These results indicated that subchronic exposure to HBCD caused a disturbance of mice metabolism, especially in TCA cycle, lipid metabolism, gut microbial metabolism, and homeostasis of amino acids, and the application of untargeted and targeted metabolomics combined with conventional toxicology approaches to evaluate the subacute effects of pollutants will provide more comprehensive information and aid in predicting health risk of these pollutants.
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PubMed
高影响因子
MOLECULES
·
2020
·Vol. 25
·期 4
·839
·
IF 3.267
Yueqing Xu,Liangxiao Zhang,Ruinan Yang,Xu Yu,Li Yu,Fei Ma,Hui Li,Xiupin Wang,Peiwu Li
Vitamin K1is one of the important hydrophobic vitamins in fat-containing foods. Traditionally, lipase is employed in the determination of vitamin K1to remove the lipids, which makes the detection complex, time-consuming, and insensitive. In this study, the determination of vitamin K1in fat-containing foods was developed based on ultrasound-assisted extraction (UAE), solid-phase extraction (SPE) combined with liquid chromatography–tandem mass spectrometry (LC-MS/MS). The optimal conditions for extraction of vitamin K1were material–liquid ratio of 1:70 (g/mL), extraction temperature of 50 °C, extraction power of 700 W, extraction time of 50 min, material-wash fluid ratio of 1:60 (g/mL), and 8 mL of hexane/anhydrous ether (97:3,v/v) as the elution solvent. Then, vitamin K1was analyzed on a ZORBAX SB-C18 column (50 mm × 2.1 mm, 1.8 μm) by gradient elution with water (0.01% formic acid) and methanol (0.01 formic acid + 2.5 mmol/L ammonium formate) as the mobile phase. The limit of detection (LOD) and limit of quantification (LOQ) were 0.05 and 0.16 μg/kg, respectively. Calibration curve was linear over the range of 10–500 ng/mL (R2> 0.9988). The recoveries at three spiked levels were between 80.9% and 119.1%. The validation and application indicated that the proposed method was simple and sensitive in determination of vitamin K1in fat-containing foods.Keywords:ultrasound-assisted extraction;solid-phase extraction;LC-MS/MS;vitamin K1;foods
研究领域:
分析化学
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营养学
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DOI
PubMed
高影响因子
BMC Chemistry
·
2023
·Vol. 17
·期 1
·1-10
·
IF 4.6
Xu Daokun,Huang Haolun,Hu Wenyan,Liu Xinmei,Yang Jun
A liquid chromatography–tandem mass spectrometry (LC–MS/MS) method was developed for the analysis of ribavirin in chicken. Samples was extracted with 0.1% formic acid and purified by Hypercarb cartridge prior to LC–MS/MS analysis. The eluates were evaporated to dryness, reconstituted in 1 mL 5mM ammonium acetate containing 5% acetonitrile (v/v) and 0.1% (v/v) formic acid. Chromatographic separation was performed on a Hypercarb analytical column under a gradient elution program with acetonitrile and 0.1% (v/v) formic acid in 5 mM ammonium acetate at a flow rate of 0.6 ml/min. The intraday and interday accuracy ranged from − 7.83 − 1.39%, and − 6.38 − 2.25%, with precisions between 1.34 − 3.88%% and 1.10 − 4.67%. The limits of detection (LODs) and limits of quantitation (LOQs) of ribavirin was 0.1 ng/mL and 0.5 ng/mL, respectively. The method was validated for linearity, accuracy, precision, matrix effect and stability. Application of the method confirmed 3 ribavirin positive samples out of 50 commercial chicken samples, with concentrations of ribavirin ranging from 0.9 μg/kg to 5.8 μg/kg a, respectively. Additionally, both AB Sciex 5500 and Agilent 6945B were proven to be suitable in ribavirin separation and quantification. The described method is suitable for the determination of ribavirin in chicken in analytical practice to monitor illegal addition of this kind of anti–viral drug.
研究领域:
分析化学
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兽药残留检测
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食品科学
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DOI
PubMed
高影响因子
MICROCHEMICAL JOURNAL
·
2023
·
IF 4.8
Shu Wang,Bingliang Zhang
Nitrilotriacetic acid (NTA) and ethylenediaminetetraacetic acid (EDTA), as widely used chelating agents, have created many environmental issues and raised much attention regarding their environmental occurrence. However, the determination of NTA and EDTA in samples of complex solution chemistry remains challenging. Here, we proposed a simple and sensitive method based on liquid chromatography tandem mass spectrometry (LC-MS/MS) to determine NTA and EDTA from aqueous samples without an enrichment step. During the analysis, H + -cation exchange was used to efficiently eliminate interference from metal ions. The intensity of NTA and EDTA with trimethylsilyldiazomethane methylation could be improved hundreds of times that of the virgin samples. To maximize sensitivity, the sample pretreatment methods, the derivatization procedures and the LC-MS/MS conditions were systematically optimized. The validated method showed low limits of quantification (0.4 μg/L for NTA and 1.5 μg/L for EDTA), a wide linear response (up to several mg/L, R 2 > 0.998), and good intra- and inter-day precision (relative standard deviation ≤ 11%). The reliability of this method was successfully validated by analysis of authentic water samples collected from three WWTPs and one river with satisfactory recoveries (80–117%). It can be proposed as a powerful analytical method of NTA and EDTA in authentic water samples and could potentially be adapted to detect other chelates and polydentate compounds.
研究领域:
环境科学
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分析化学
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DOI
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2024
·
IF 3.8
Lei Zhang,Xu Liu,Tenghui Jin,Jing Dong,Xiaodong Li,Youyi Zhang,Dongyang Liu
Some bile acids (BAs) were considered as biomarkers or have therapeutical effect on metabolic diseases. However, due to the existence of isomers and limitations in sensitivity, simultaneous quantification of multiple BAs remains a challenge. The aim of this study is to establish an accurate and sensitive method for the determination of multiple BAs with similar polarity. A LC-MS/MS analytical method capable of quantifying forty-five BAs simultaneously using nine stable isotope internal standards was developed and fully validated based on key isomers-oriented separation strategy. The method was further applied to analyze plasma samples to describe the dynamic profile of BAs after high glucose intake. The chromatography and mass spectrum conditions were optimized to enable the accurate quantification of forty-five BAs, while ensuring the lower limit of quantification between 0.05–10 ng/mL. The results of system suitability, linearity, dilution integrity, accuracy and precision demonstrated the good quantitative capacity and robustness of the method. A total of thirty-five BAs were quantified in plasma samples from twelve healthy Chinese individuals. The established method featured superior sensitivity and better separation efficiency compared to previous studies. Meanwhile, BAs exhibited correlations with glucose and insulin, suggesting their potential as biomarkers for metabolic disorders.
研究领域:
分析化学
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生物化学
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代谢组学
·
临床化学
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DOI
PubMed
高影响因子
SCIENCE OF THE TOTAL ENVIRONMENT
·
2023
·
IF 9.8
Yuling Zhong,Chenzhi Hou,Xinyi Gao,Mingyu Wang,Yan Yao,Mengyi Chen,Bin Di,Mengxiang Su
The illegal use of beta-agonists could cause severe problems to human health. In this study, the usage of beta-agonists in 31 cities across China was estimated using wastewater-based epidemiology (WBE). The proposed method is based on solid-phase extraction (SPE) and LC-MS/MS and was developed and validated to determine the concentration of seven beta-agonists in wastewater. A population model based on cotinine (COT), NH 4 -N and the flow volume was constructed to estimate the population equivalents for different wastewater treatment plants (WWTPs). Clenbuterol and ractopamine are banned in China for both animal husbandry and medical use, but were nevertheless detected in some wastewater samples at rates of 6.2 % and 4.7 %, respectively ( n = 339). The WBE-based consumption of clenbuterol and ractopamine were compared with the acceptable daily intake (ADI) and the health risks were assessed by their hazard quotients (0.26–6.62 for clenbuterol and 9.27 × 10 −4 -0.05 for ractopamine). Salbutamol, clorprenaline and terbutaline were observed in practically all wastewater samples at concentrations of up to several ng/L, whereas the formoterol and bambuterol concentrations were below the detection limit in all samples. Salbutamol consumption (7.35 ± 4.14 mg/1000 inh/day) was highest among the examined beta-agonists and varied regionally. Beta-agonist consumption based on WBE was higher in some cities than that based on medical survey data, indicating potential illegal use. These results show that WBE can be a straightforward and supplementary method for monitoring beta-agonist usage at the population level and spatially.
研究领域:
环境科学
·
流行病学
·
公共卫生
·
分析化学
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DOI
PubMed
高影响因子
Frontiers in Immunology
·
2024
·
IF 5.7
Li Na,Wang Tianyi,Zhang Huiying,Li Xiao,Bai Haochen,Lu Ning,Lu Kaizhi
Objective: This investigation sought to delineate the causal nexus between plasma glutamine concentrations and leukemia susceptibility utilizing bidirectional Mendelian Randomization (MR) analysis and to elucidate the metabolic ramifications of asparaginase therapy on glutamine dynamics in leukemia patients.Methods: A bidirectional two-sample MR framework was implemented, leveraging genetic variants as instrumental variables from extensive genome-wide association studies (GWAS) tailored to populations of European descent. Glutamine quantification was executed through a rigorously validated Liquid Chromatography-Mass Spectrometry/Mass Spectrometry (LC-MS/MS) protocol. Comparative analyses of glutamine levels were conducted across leukemia patients versus healthy controls, pre- and post-asparaginase administration. Statistical evaluations employed inverse variance weighted (IVW) models, MR-Egger regression, and sensitivity tests addressing pleiotropy and heterogeneity.Results: The MR findings underscored a significant inverse association between glutamine levels and leukemia risk (IVW p = 0.03558833), positing lower glutamine levels as a contributory factor to heightened leukemia susceptibility. Conversely, the analysis disclosed no substantive causal impact of leukemia on glutamine modulation (IVW p = 0.9694758). Notably, post-asparaginase treatment, a marked decrement in plasma glutamine concentrations was observed in patients (p = 0.0068), underlining the profound metabolic influence of the therapeutic regimen.Conclusion: This study corroborates the hypothesized inverse relationship between plasma glutamine levels and leukemia risk, enhancing our understanding of glutamine’s role in leukemia pathophysiology. The pronounced reduction in glutamine levels following asparaginase intervention highlights the critical need for meticulous metabolic monitoring to refine therapeutic efficacy and optimize patient management in clinical oncology. These insights pave the way for more tailored and efficacious treatment modalities in the realm of personalized medicine.
研究领域:
医学
·
遗传学
·
代谢组学
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DOI
PubMed
高影响因子
CLINICA CHIMICA ACTA
·
2021
·
IF 3.786
Qian Gong,Xiuming Zhang,Aifeng Liang,Sinian Huang,Guangang Tian,Mengjiao Yuan,Qing Ke,Yijun Cai,Bin Yan,Jin Wang,Jinjin Wang
Background and aims Colorectal cancer (CRC) is part of the most widespread malignant tumors. At present, colonoscopy is a routine procedure in the diagnosis of CRC, but it is traumatic. Carcinoembryonic antigen, CA199, and CA242 are common serum markers for the diagnosis of CRC; however, they do not demonstrate satisfactory specificity and sensitivity for the diagnosis of CRC. Hence, Now it is necessary to screen many valuable serum biomarkers for CRC, proteomics methods have been used to investigate PTMs such as glycosylation of proteins with prominent roles in the occurrence and development of tumors. Methods This study screens altering glycosylated proteins of CRC tissues using LC-MS/MS quantitative glycoproteomics, and then these candidate biomarkers for CRC are further validated by serum glycoproteomics. Results The results of glycoproteomics in CRC tissues show that the abundance of 160 and 79 glycerogelatin proteins was obviously upregulated and downregulated compared with their adjacent tissues( P < 0.05). Bioinformatics analysis suggests that these molecules are mainly involved in many biological processes, including skeletal system development, collagen fibril organization, and receptor-mediated endocytosis. Results of serum glycoproteomics show that the changing trends of 2 protein glycosylation were consistent with MS results of CRC tissues, including ICAM1and APMAP. Areas under the ROC curve (AUC) results confirm that ICAM1and APMAP as early immune diagnosis markers of CRC has excellent sensitivity and specificity. Conclusion The ICAM1 and APMAP may serve as a potential tumor marker for CRC.
研究领域:
肿瘤学
·
蛋白质组学
·
医学
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DOI
PubMed
高影响因子
INTERNATIONAL JOURNAL OF MOLECULAR SCIENCES
·
2024
·Vol. 26
·期 1
·77
·
IF 4.9
Zhiting Guo,Huiyan Yu,Kexin Yang,Wenjing Feng,Miao Liu,Tao Wang,Rong Xiao
Oxysterols, as metabolites of cholesterol, play a key role in cholesterol homeostasis, autophagosome formation, and regulation of immune responses. Disorders in oxysterol metabolism are closely related to the pathogenesis of neurodegenerative diseases. To systematically investigate the profound molecular regulatory mechanisms of neurodegenerative diseases, it is necessary to quantify oxysterols and their metabolites in central and peripheral biospecimens simultaneously and accurately. However, there are a lot of unsolved problems with the existing methods, such as the hindrance of applying a single method to different biological specimens or the challenge of simultaneous quantification due to differential groups on the ends of the oxysterol side chains. Herein, according to the physicochemical properties and structure of oxysterols, an optimized liquid chromatography-tandem mass spectrometry method for the quantification of oxysterols was established by optimizing the sample preparation process, chromatographic conditions, mobile phase pH, and solvent selection. Seven oxysterols were detected by this method, including 27-hydroxycholesterol, 7α-hydroxycholesterol, 7α,27-dihydroxycholesterol, 7-dehydrocholesterol, 7α-hydroxy-3-oxo-4-cholestenoic acid, 3-hydroxy-5-cholestenoic acid, and 24(S)-hydroxycholesterol. Non-derivatization extraction with methyl tert-butyl ether was used for different biospecimens, followed by simultaneous chromatographic separation of oxysterols on a phenyl hexyl column. By repeated validation, this method exhibited satisfactory linearity, precision, recovery, sensitivity, repeatability, and stability, and it was successfully applied to the detection of oxysterols in the plasma, cerebral cortex, and liver of mouse. In summary, our optimized method enables concurrent analysis and quantification of oxysterols and their metabolites in various biospecimens, presenting a broad range of applicability.
研究领域:
生物化学
·
医学分析
·
神经科学
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DOI
PubMed
高影响因子
危险品化学品经营许可证（带存储）