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MICROCHIMICA ACTA · 2021 ·Vol. 188 ·期 10 ·1-10 · IF 5.833

Competitive immune-nanoplatforms with positive readout for the rapid detection of imidacloprid using gold nanoparticles

Chen He,Sun Wanlin,Zhang Zhongrong,Tao Zhexuan,Qin Yuling,Ding Yuan,Wang Limin,Wang Minghua,Hua Xiude

Two high-sensitivity competitive immune-nanoplatforms based on the inner filter effect (IFE-IN) and magnetic separation (MS-IN) with a positive readout were developed to rapidly detect imidacloprid (IMI) using gold nanoparticles (AuNPs). For IFE-IN, IMI competes with AuNPs-labeled IMI antigens (IMI-BSA-AuNPs) to bind with anti-IMI monoclonal antibody (mAb)-conjugated NaYF 4 :Yb,Er upconversion nanoparticles, which changes the fluorescence signal at excitation/emission wavelength of 980/544 nm. For MS-IN, the immunocomplex of IMI-BSA-AuNPs and magnetic-nanoparticles-labeled mAb (mAb-MNPs) dissociates in the presence of IMI, and the optical density of IMI-BSA-AuNPs at 525 nm increases with the IMI concentration after magnetic separation. Under the optimal conditions, the IMI concentration producing a 50% saturation of the signal (SC 50 ) and linear range (SC 10 − SC 90 ) were found to be 4.30 ng mL −1 and 0.47 − 21.37 ng mL −1 for IFE-IN, while 1.21 ng mL −1 and 0.07 − 10.21 ng mL −1 for MS-IN, respectively. Both IFE-IN and MS-IN achieved excellent accuracy for the detection of IMI in different matrices. The quantities of IMI in apple samples detected by IFE-IN and MS-IN were consistent with the high-performance liquid chromatography results. Graphical abstract For IFE-IN, analyte competes with AuNPs-labeled-antigen to bind with the mAb-conjugated-UCNPs, which changes the fluorescence signal at 544 nm. For MS-IN, the immunocomplex of AuNPs-labeled-antigen and mAb-conjugated-MNPs dissociates in the presence of analyte, and the optical density of AuNPs-labeled-antigen at 525 nm increases with increasing analyte concentration after separation.

研究领域: 分析化学 · 纳米技术 · 环境科学 · 食品安全
✓ 已验证 产品关联 DOI PubMed 高影响因子
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Analytical Methods · 2020 ·Vol. 12 ·期 17 ·2221-2227 · IF 2.596

LC-MS in combination with DMBA derivatization for sialic acid speciation and distribution analysis in fish tissues

Junjie Du,Qiwei Zhang,Jianjun Li,Qi Zheng

Sialic acid (Sia) is widespread in vertebrates and humans as well as in some microbes and invertebrates. It is well known that O-acetylation is a common modification for Sia. Also, highly O-acetylated Sias have been reported in humans, bovines, and fish. Derivatization based on 1,2-diamino-4,5-methylenedioxybenzene (DMB) coupled with LC-fluorescence detection or LC-MS analysis has been the routine analytical strategy for O-acetylation profiling of Sias. Unfortunately, DMB offers poor chromatographic resolution for some O-acetylated species. Herein, we report another derivatization reagent, 4,5-dimethylbenzene-1,2-diamine (DMBA), for the LC-MS analysis of Sia isomers. The DMBA method was first evaluated using Sia reference standard, horse serum and carp blood. The results demonstrate that DMBA provides superior chromatographic separation efficiency and comparable MS/MS spectra to DMB. The proposed method was then applied to the analysis of relative abundance of each Sia species in fish tissues, including liver, intestine, muscle and brain. It was found that the relative amounts of Sia species were significantly different among the four tissues. Thus, DMBA derivatization-based LC-MS methods have great potential in investigating the O-acetylation level of Sias in various samples, such as human food and bio-pharmaceutical products.

CAS / MDL: 64-17-5 103-83-3 76-05-1
研究领域: 分析化学 · 生物化学 · 药学
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Bioanalysis · 2023 ·Vol. 15 ·期 6 · IF 1.8

Simultaneous assaying of NLG919, tryptophan and kynurenine by ultra-high performance LC–MS in pharmacokinetics and biodistribution studies

Juan Li,Yongjing Cao,Xiaojie Zhang,Min An,Juntao Zhang,Yanhua Liu

Background: Indocyanine2,3-dioxygenase (IDO) is an enzyme that can catalyze the metabolism of tryptophan (Trp) into kynurenine (Kyn), thus inhibiting the tumor immune microenvironment. Method: Based on its inhibitor, NLG919 (NLG), the authors developed a new immunomodulatory polymer micelle and established and verified an ultrahigh performance liquid chromatography–mass spectrometry method for the simultaneous determination of NLG, Trp and Kyn in mouse tumors through the ratio determination of Trp/Kyn tissue distribution and pharmacokinetics. The linear range of the method was 0.001–10 μg/ml. Results: Compared with NLG solution, the immunomodulatory polymeric drug-loaded micelles based on polystyrene-arginine showed higher Trp/Kyn ratio, more tumor aggregation and good pharmacokinetics. Conclusion: This method has been successfully applied to the simultaneous determination of Trp/Kyn and NLG in tumor tissues of mice.

研究领域: 药理学 · 肿瘤学 · 分析化学 · 生物技术
✓ 已验证 DOI PubMed 高影响因子
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Forensic Toxicology · 2016 ·Vol. 34 ·期 2 ·398-402 · IF 0

Successful quantification of 4′-methyl-α-pyrrolidinohexanophenone (MPHP) in human urine using LC–TOF-MS in an autopsy case

Shintani-Ishida Kaori,Kakiuchi Yasuhiro,Ikegaya Hiroshi

The toxicological detection of the new synthetic cathinone 4′-methyl-α-pyrrolidinohexanophenone (MPHP) in urine samples has been impossible, because much of MPHP is metabolized before its excretion into urine. In this study, we successfully quantified unmetabolized MPHP in urine of an autopsy case using a sensitive method by liquid chromatography–time-of-flight-mass spectrometry. The quantification method showed good linearity in the range of 1.00–100 ng/mL, and the limit of detection was 0.5 ng/mL in human urine. In the autopsy case, the concentrations of MPHP in urine, plasma, and liver tissue samples were determined to be 60.1, 32.9 ng/mL, and 63.1 ng/g, respectively.

研究领域: 法医学 · 分析化学 · 毒理学
✓ 已验证 DOI PubMed
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American Journal of Translational Research · 2021 · IF 4.06

Application value of UPLC-MS/MS in detecting serum concentration of anti-schizophrenic drugs in patients with mental illnes

Shaochang Wu,Guidong Zhu,Dajin Zhou,Hongtao Xu,Longyou Zhao

Objective: This study was designed to demonstrate the accuracy of ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) in detecting serum concentration of anti-schizophrenic drugs in patients with mental illness. Methods: The study participants were 186 schizophrenia patients treated in our hospital. Serum concentrations of anti-schizophrenic drugs in Chinese patients with mental illness were evaluated according to the reference intervals of drug therapy recommended in the guidelines. Results: Five drugs, namely Aripiprazole (ARI), Amisulpride (AMI), Olanzapine (OLA), Paliperidone (PAL) and Ziprasidone (ZIP) all showed good linearity within the linear range. The within-day precision of the above five drugs was all between 1.3%-8.9% and the inter-day precision was between 1.8%-7.6%, with within-day and inter-day relative standard deviations (RSDs) less than 15.00% and accuracy ranging from 87.00% to 106.73%. However, AMI had a mean blood concentration of 436.31±241.05 ng/mL (median concentration: 379.34 ng/mL), which was significantly higher than the reference range (100-320 ng/mL) recommended in the guidelines. Good recovery rates (86.21%-99.77%) were obtained after the samples were stored at room temperature for 24 h, at 4°C for 48h and at -20°C for half a year. Conclusions: Given that UPLC-MS/MS renders more accurate results in detecting the concentration of psychotropic drugs, it can be applied clinically to detect the concentration of therapeutic drugs in patients with mental illness.

CAS / MDL: 64-18-6
研究领域: 临床医学 · 药理学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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INTERNATIONAL JOURNAL OF MOLECULAR SCIENCES · 2024 ·Vol. 25 ·期 7 ·3654 · IF 4.9

Unveiling Anti-Diabetic Potential of Baicalin and Baicalein from Baikal Skullcap: LC–MS, In Silico, and In Vitro Studies

Wencheng Zhao,Huizi Cui,Kaifeng Liu,Xiaotang Yang,Shu Xing,Wannan Li

Type 2 diabetes mellitus (T2DM) is marked by persistent hyperglycemia, insulin resistance, and pancreatic β-cell dysfunction, imposing substantial health burdens and elevating the risk of systemic complications and cardiovascular diseases. While the pathogenesis of diabetes remains elusive, a cyclical relationship between insulin resistance and inflammation is acknowledged, wherein inflammation exacerbates insulin resistance, perpetuating a deleterious cycle. Consequently, anti-inflammatory interventions offer a therapeutic avenue for T2DM management. In this study, a herb called Baikal skullcap, renowned for its repertoire of bioactive compounds with anti-inflammatory potential, is posited as a promising source for novel T2DM therapeutic strategies. Our study probed the anti-diabetic properties of compounds from Baikal skullcap via network pharmacology, molecular docking, and cellular assays, concentrating on their dual modulatory effects on diabetes through Protein Tyrosine Phosphatase 1B (PTP1B) enzyme inhibition and anti-inflammatory actions. We identified the major compounds in Baikal skullcap using liquid chromatography–mass spectrometry (LC–MS), highlighting six flavonoids, including the well-studied baicalein, as potent inhibitors of PTP1B. Furthermore, cellular experiments revealed that baicalin and baicalein exhibited enhanced anti-inflammatory responses compared to the active constituents of licorice, a known anti-inflammatory agent in TCM. Our findings confirmed that baicalin and baicalein mitigate diabetes via two distinct pathways: PTP1B inhibition and anti-inflammatory effects. Additionally, we have identified six flavonoid molecules with substantial potential for drug development, thereby augmenting the T2DM pharmacotherapeutic arsenal and promoting the integration of herb-derived treatments into modern pharmacology.

CAS / MDL: 50-78-2
研究领域: 药理学 · 糖尿病研究 · 草药医学 · 生物化学 · 分子生物学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS · 2022 · IF 3.571

Quantitative analysis of 20 purine and pyrimidine metabolites by HILIC-MS/MS in the serum and hippocampus of depressed mice

Zhenyao Lu,Sijia Li,Nan Aa,Yuanmao Zhang,Ran Zhang,Chen Xu,Shize Zhang,Xiangqing Kong,Guangji Wang,Jiye Aa,Yue Zhang

Purine and pyrimidine metabolism are vital metabolic pathways in the development, proliferation or repairment of cells or tissues associated with various diseases. Here, a simple, all-in-one injection hydrophilic interaction liquid chromatography-tandem mass spectrometry method was developed for simultaneous determination of 20 metabolites: adenine , adenosine, deoxyadenosine , adenosine 5′-monophosphate, cyclic adenosine monophosphate, hypoxanthine , xanthine , inosine , deoxyinosine , xanthosine , xanthosine 5′-monophosphate and uric acid , which are products of purine metabolism; uridine , deoxyuridine , uridine 5′-monophosphate and uracil , are products of pyrimidine metabolism; and corticosterone , methionine , acetylcholine and serotonin. To minimize interference of endogenous molecules in sample matrixes, a combination of activated carbon adsorption and a serum substitute matrix (5% bovine serum albumin in phosphate buffered saline) was utilized and jointly applied. The sensitivity, linearity, stability, precision, accuracy and extraction recovery were evaluated, and the method was demonstrated to be accurate, sensitive and reliable. An analytical strategy was successfully applied to quantitatively determine 20 metabolite levels in the serum and hippocampus of mice with chronic social defeat stress-induced depression. The results showed greatly perturbed purine metabolism in the depressed mice, which was primarily characterized by dramatic increases in hypoxanthine, xanthine and inosine in serum and reduced levels of adenine, adenosine and adenosine 5′-monophosphate in the hippocampus. These findings suggest that this novel strategy can facilitate the quantitative analysis of adenine and other purine and pyrimidine metabolites in tissue and serum and exhibits great potential in the exploration of metabolism-related mechanisms of relevant diseases.

研究领域: 生物化学 · 医学 · 神经科学
✓ 已验证 DOI 高影响因子
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Foods · 2024 ·Vol. 13 ·期 20 ·3286 · IF 4.7

Simultaneous and High-Throughput Analytical Strategy of 30 Fluorinated Emerging Pollutants Using UHPLC-MS/MS in the Shrimp Aquaculture System

Di Huang,Chengbin Liu,Huatian Zhou,Xianli Wang,Qicai Zhang,Xiaoyu Liu,Zhongsheng Deng,Danhe Wang,Yameng Li,Chunxia Yao,Weiguo Song,Qinxiong Rao

This study established novel and high-throughput strategies for the simultaneous analysis of 30 fluorinated emerging pollutants in different matrices from the shrimp aquaculture system in eastern China using UHPLC-MS/MS. The parameters of SPE for analysis of water samples and of QuEChERS methods for sediment and shrimp samples were optimized to allow the simultaneous detection and quantitation of 17 per- and polyfluoroalkyl substances (PFASs) and 13 fluoroquinolones (FQs). Under the optimal conditions, the limits of detection of 30 pollutants for water, sediment, and shrimp samples were 0.01–0.30 ng/L, 0.01–0.22 μg/kg, and 0.01–0.23 μg/kg, respectively, while the limits of quantification were 0.04–1.00 ng/L, 0.03–0.73 μg/kg, and 0.03–0.76 μg/kg, with satisfactory recoveries and intra-day precision. The developed methods were successfully applied to the analysis of multiple samples collected from aquaculture ponds in eastern China. PFASs were detected in all samples with concentration ranges of 0.18–0.77 μg/L in water, 0.13–1.41 μg/kg (dry weight) in sediment, and 0.09–0.96 μg/kg (wet weight) in shrimp, respectively. Only two FQs, ciprofloxacin and enrofloxacin, were found in the sediment and shrimp. In general, this study provides valuable insights into the prevalence of fluorinated emerging contaminants, assisting in the monitoring and control of emerging contaminants in aquatic foods.

CAS / MDL: 631-61-8 308068-56-6
研究领域: 环境科学 · 分析化学 · 水产养殖学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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STEROIDS · 2015 · IF 2.639

A new quantitation method of protodioscin by HPLC–ESI-MS/MS in rat plasma and its application to the pharmacokinetic study

Xinxin Zhang,Zengjun Guo,Jing Li,Yoichiro Ito,Wenji Sun

A specific high performance liquid chromatography tandem mass spectrometry (HPLC–MS/MS method) was established for determining the concentration of protodioscin (PG) in rat plasma after intragastric administration of its standard form. Ginsenoside Rb 1 was selected as the internal standard (IS). The plasma sample was prepared using one-step deproteinization procedure by adding three parts of acetonitrile to precipitate proteins. The chromatographic separation was accomplished on an Inersil ODS-3 C 18 column (250   ×   4.6   mm, 5   μm) with a mobile phase composed with acetonitrile and water containing 0.1% formic acid under a gradient elution mode at a flow rate of 1   mL   min −1 . A 3:1 portion of the eluent after a microsplit was detected on a triple quadrupole tandem mass spectrometer coupled with electrospray ionization (ESI) in positive ion and multiple reaction monitoring (MRM) scanning modes. The mass transitions were selected as 888.1   →   1050.2 for PG and 948.2   →   1110.3 for IS, respectively. After careful validation, the plasma samples were always stable under different storage conditions. These analytical results rendered sensitive, selective, and reliable values by this established method which displayed high accuracy, adequate extracted recoveries, and almost negligible matrix effects. This method was applied to the pharmacokinetic studies on PG level in the rat plasma and its pharmacokinetic effect. The results of our studies suggest that the present method may be a useful tool for further clinical study of PG.

CAS / MDL: 64-18-6
研究领域: 分析化学 · 药物代谢 · 生物医学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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ANALYTICAL LETTERS · 2024 · IF 1.6

Rapid Determination of Flavorings in e-Cigarette Liquid by Direct Analysis in Real Time (DART) Mass Spectrometry (MS) in the Quick Strip Mode

Xuerui Lou,Minglei Li,Weiwei Guo,Yingjie Fu,Hui Xi,Peng Li,Wuduo Zhao,Shihao Sun

Electronic cigarettes (E-cigarettes) have become popular around the world. An important reason is the variety of available flavors. However, many countries have imposed restrictions on flavor substances in E-cigarettes due to their potential health risks. Therefore, it is necessary to develop an effective way to identify flavorings in E-cigarette liquids. In this work, direct analysis in real time-mass spectrometry (DART-MS) in the quick strip (QS) mode was developed and applied to determine flavorings in the E-cigarettes. Vanillin, ethyl vanillin, maltol, and ethyl maltol were quantified. Meanwhile, the ionization efficiency of flavorings in the different solvents was compared in the QS mode, which revealed that the solvent boiling point was related to the analyte ionization efficiency. The effect of endogenous matrix (propylene glycol and glycerol) on flavoring ionization was also investigated. Calibration curves with satisfactory linearity (R2 > 0.99) were established from 1 to 1000 μg L−1. Good sensitivity (limits of detection [LODs] < 0.3 μg L−1), recoveries (92.6% to 104.7%), and acceptable repeatability (relative standard deviations < 14.6%, n = 5) were obtained. The limits of quantification (LOQs; 10–50 μg g−1) for the E-cigarette liquid sample were much lower than the regulatory limits. The developed method provided a simple way for rapidly determining flavorings in E-cigarettes.

研究领域: 分析化学 · 公共卫生 · 毒理学
✓ 已验证 产品关联 DOI 高影响因子
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Food Science and Human Wellness · 2024 · IF 5.6

Application of solid-phase extraction and gas chromatography-mass spectrometry (SPE-GC-MS) in resolution of metabolism pattern of higher alcohols in rat plasma

Yufei Liu,Xiaonian Cao,Zhilei Zhou,Qingxi Ren,Zhongwei Ji,Min Gong,Yuezheng Xu,Weibiao Zhou,Shuguang Chen,Jian Mao

Higher alcohols are key factors affecting sensory quality and post-drinking comfort of alcoholic beverages. A strategy combining solid-phase extraction and gas chromatography-mass spectrometry (SPE-GC-MS) was established to analyze the metabolism pattern of higher alcohols in rat plasma after gavage of 4 common alcoholic beverages including huangjiu, baijiu, wine and brandy. 7 mL of dichloromethane was determined as the optimal extraction condition, and 8 higher alcohols were precisely quantified with detection limits of 1.82−11.65 μg/L, recoveries of 89.07 %−110.89 % and fine repeatability. The fastest absorption and elimination rates of plasma total higher alcohols were observed in baijiu and huangjiu group, respectively, and the highest peak concentration was found in brandy group. Additionally, the metabolic rate of plasma isoamyl alcohol in huangjiu group was faster than that in wine group at the same intragastric administration dosage. This study may provide potential insight for evaluation of alcoholic beverage quality.

CAS / MDL: 75-09-2 67-56-1
研究领域: 分析化学 · 食品科学 · 代谢生物学
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Analytical Methods · 2023 ·Vol. 15 ·期 26 ·3206-3224 · IF 3.1

A comprehensive and high-throughput screening method for multiple prohibited substances by UPLC-QE Plus-HRMS and HPLC-QQQ-MS in human urine for doping control

Yunxi Liu,Tianyu Dong,Kuan Yan,Zhanliang Wang,Genye He,Yufeng Zhang,Congcong Ma,Lu Liu,Wei Chang,Lisi Zhang

Since the World Anti-Doping Agency's (WADA) Prohibited List is updated on an annual basis, screening methods must be continually adapted to align with these changes. In accordance with Technical Document-MRPL 2022, a newly combined, comprehensive, rapid and high-throughput doping control screening method has been developed for the analysis of 350 substances with different polarities in human urine using ultra-high performance liquid chromatography coupled with Q Exactive Plus Hybrid Quadrupole-Orbitrap mass spectrometer (UPLC-QE Plus-HRMS) and ultra-high performance liquid chromatography coupled with triple quadrupole mass spectrometer (UPLC-QQQ-MS). The limits of detection were in the range of 0.12–50 ng mL−1 for beta-2 agonists, hormone and metabolic modulators, narcotics, cannabinoids and glucocorticoids, 0.1–14 ng mL−1 for the manipulation of blood and blood components, beta blockers, anabolic agents and hypoxia-inducible factor (HIF) activating agents, and 2.5–100 000 ng mL−1 for substances of Appendix A, diuretics & masking agents and stimulants. The sample preparation consisted of two parts: one is the dilute & shoot part analyzed in UPLC-QQQ-MS, another is a mixture of the dilute & shoot part and a liquid–liquid extraction part of hydrolyzed human urine analyzed in UPLC-QE Plus-HRMS in full scan mode with polarity switching and parallel reaction monitoring (PRM) mode. The method has been fully validated for doping control purposes. All the substances were compliant with WADA's required 1/2 minimum requirement performance level (MRPL) or minimum reporting level (MRL), and this method was successfully used in the 2022 Beijing Winter Olympic Games and Winter Paralympic Games for anti-doping purpose.

研究领域: 分析化学 · 运动科学 · 药理学 · 法医学
✓ 已验证 DOI PubMed 高影响因子
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