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Simultaneous determination of indole metabolites of tryptophan in rat feces by chemical labeling assisted liquid chromatography-tandem mass spectrometry

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Chinese Chemical Letters 2022年第11期33卷 4746-4749页

作者： Qin-Feng Zhang Hua-Ming Xiao Jin-Tao Zhan Bi-Feng Yuan Yu-Qi Feng Department of Chemistry Wuhan UniversityWuhan 430072China School of Public Health Wuhan UniversityWuhan 430071China

As the connecting part of diet and host physiology,intestinal microbes can convert the ingested diet into a huge number of physiologically active small molecules.Indole metabolites of tryptophan are precursors or signal molecules for many biologically active substances,which are involved in serotonin and microbial catabolism pathways.To understand the influence of tryptophan metabolism in the intestinal environment on the neurological and immune systems at the molecular level,it is important to establish a high-coverage analytical method to comprehensively analyze the metabolites involved in tryptophan metabolism.However,due to a small molecular weight and poor response during mass spectrometry analysis,as well as weak retention on the reversed-phase chromatography,determination of indole metabolites of tryptophan is challenging.Here,we proposed a method for the simultaneous determination of 20 indole metabolites of tryptophan in a single run on reversed-phase chromatography by chemical labeling coupled to liquid chromatography-tandem mass spectrometry analysis.4-(Dimethylamino)benzaldehyde(DMAB)was used for the labeling of indole metabolites of tryptophan,which could significantly improve the detection sensitivities and retention of these metabolites on reversed-phase chromatography.With the developed method,we realized the sensitive detection and comprehensive analysis of 15 endogenous indole metabolites of tryptophan in rat feces samples with functional dyspepsia intervention by acupuncture.The developed method offers a useful tool for studying tryptophan metabolism-related diseases.

关键词： Chemical labeling Liquid chromatography-mass spectrometry Indole metabolites Tryptophan Rat feces

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Insight into chemical basis of traditional Chinese medicine based on the state-of-the-art techniques of Liquid chromatography-mass spectrometry

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Acta Pharmaceutica Sinica B 2021年第6期11卷 1469-1492页

作者： Yang Yu Changliang Yao De-an Guo Shanghai Research Center for Modernization of Traditional Chinese Medicine National Engineering Laboratory for TCM Standardization TechnologyShanghai Institute of Materia MedicaChinese Academy of SciencesShanghai 201203China University of Chinese Academy of Sciences Beijing 100049China

Traditional Chinese medicine(TCM) has been an indispensable source of drugs for curing various human diseases.However,the inherent chemical diversity and complexity of TCM restricted the safety and efficacy of its usage.Over the past few decades,the combination of liquid chromatography with mass spectrometry has contributed greatly to the TCM qualitative analysis.And novel approaches have been continuously introduced to improve the analytical performance,including both the data acquisition methods to generate a large and informative dataset,and the data post-processing tools to extract the structure-related MS information.Furthermore,the fast-developing computer techniques and big data analytics have markedly enriched the data processing tools,bringing benefits of high efficiency and accuracy.To provide an up-to-date review of the latest techniques on the TCM qualitative analysis,multiple data-independent acquisition methods and data-dependent acquisition methods(precursor ion list,dynamic exclusion,mass tag,precursor ion scan,neutral loss scan,and multiple reaction monitoring)and post-processing techniques(mass defect filtering,diagnostic ion filtering,neutral loss filtering,mass spectral trees similarity filter,molecular networking,statistical analysis,database matching,etc.) were summarized and categorized.Applications of each technique and integrated analytical strategies were highlighted,discussion and future perspectives were proposed as well.

关键词： Liquid chromatography-mass spectrometry Qualitative analysis Traditional Chinese medicine Data acquisition Data post-processing

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Comprehensive profiling and evaluation of the alteration of RNA modifications in thyroid carcinoma by liquid chromatography-tandem mass spectrometry

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Chinese Chemical Letters 2022年第8期33卷 3772-3776页

作者： Meng-Yuan Chen Chu-Bo Qi Xiao-Meng Tang Jiang-Hui Ding Bi-Feng Yuan Yu-Qi Feng School of Public Health Wuhan UniversityWuhan 430071China Department of Chemistry Sauvage Center for Molecular SciencesWuhan UniversityWuhan 430072China Jiangxi Provincial People's Hospital Affiliated to Nanchang University Nanchang 330006China

RNA molecules contain diverse modifications that display important functions in a variety of physiological and pathological processes.So far over 150 chemical modifications have been characterized to be present in various RNA species,such as in messenger RNA(mRNA),ribosomal RNA(rRNA),and transfer RNA(tRNA).Previous studies revealed that certain RNA modifications were correlated to specific human diseases,indicating RNA modifications could serve as the potential indicator of human diseases.However,systemic investigation of the alteration of RNA modifications in different RNA species of carcinoma tissues are still lacked.Herein,we carried out the comprehensive profiling and evaluation of the alteration of RNA modifications in thyroid carcinoma by liquid chromatography-tandem mass spectrometry(LC-ESIMS/MS)analysis.The developed method allowed us to simultaneously detect 48 different types of RNA modifications.Using this method,we detected 10,15,14,and 25 modifications in m RNA,18 S r RNA,28 S rRNA and small RNA(<200 nt),respectively.Compared to the normal tissues,we revealed a total of 14 RNA modification exhibited significant increase and 2 RNA modifications showed significant decrease in thyroid carcinoma tissues.Our study provided the first comprehensive profile as well as the alteration of modifications in different RNA species in thyroid carcinoma and matched tumor-adjacent normal tissues.The altered pattern RNA modifications may serve as the indicator of thyroid carcinoma.Moreover,this study may promote the in-depth understanding of the regulatory roles of RNA modifications in thyroid carcinoma.

关键词： RNA modification Liquid chromatography-mass spectrometry Thyroid carcinoma Profiling

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Recent progress in polar metabolite quantification in plants using Liquid chromatography-mass spectrometry

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Journal of Integrative Plant Biology 2014年第9期56卷 816-825页

作者： Zhiqian Liu Simone Rochfort Department of Environment and Primary Industries Dairy Futures Co-operative Research Centre La Trobe University

Metabolite analysis or metabolomics is an important component of systems biology in the post-genomic era.Although separate liquid chromatography（LC） methods for quantification of the major classes of polar metabolites of plants have been available for decades,a single method that enables simultaneous determination of hundreds of polar metabolites is possible only with gas chromatography-mass spectrometry（GC-MS） techniques.The rapid expansion of new LC stationary phases in the market and the ready access of mass spectrometry in many laboratories provides an excellent opportunity for developing LC-MS based methods for multitarget quantification of polar metabolites.Although various LC-MS methods have been developed over the last 10 years with the aim to quantify one or more classes of polar compounds in different matrices,currently there is no consensus LC-MS method that is widely used in plant metabolomics studies.The most promising methods applicable to plant metabolite analysis will be reviewed in this paper and the major problems encountered highlighted.The aim of this review is to provide plant scientists,with limited to moderate experience in analytical chemistry,with up-to-date and simplified information regarding the current status of polar metabolite analysis using LC-MS techniques.

关键词： Aqueous normal phase chromatography hydrophilic interaction liquid chromatography Liquid chromatography-mass spectrometry plants polar metabolites

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Discrimination and Quantification of True Biological Signals in Metabolomics Analysis Based on Liquid chromatography-mass spectrometry

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Molecular Plant 2016年第8期9卷 1217-1220页

作者： Duan, Lixin Molnar, Istvan Snyder, John Hugh Shen, Guo-an Qi, Xiaoquan Chinese Acad Sci Inst Bot Key Lab Plant Mol Physiol 20 NanxincunXiangshan Rd Beijing 100093 Peoples R China Univ Arizona Nat Prod Ctr Sch Nat Resources & Environm 250 East Valencia Rd Tucson AZ 85706 USA

Dear Editor Metabolomics is a rapidly emerging field of post-genomic research that aims to comprehensively analyze all metabolites in biological samples. Potential biomarkers that distinguish prostate cancer samples were successfully identified through metabolomics analysis （Sreekumar et al., 2009）. Metabolome quantitative trait loci （mQTL） and genome-wide association studies coupled with metabolomics analysis （mGWAS） also became efficient tools to decipher the genetic basis of complex metabolic traits in large populations （Gong et al., 2013; Chen et al., 2014）.

关键词： Liquid chromatography-mass spectrometry METABOLOMICS

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Analysis of chloramphenicol in honey by on-line pretreatment liquid chromatography-tandem mass spectrometry

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Chinese Chemical Letters 2015年第1期26卷 36-38页

作者： Shin-ichi Kawano Hong-Yuan Hao Yuki Hashi Jin-Ming Lin Department of Chemistry Beijing Key Laboratory of Microanalytical Methods and InstrumentationTsinghua University Shimadzu Global COE for Application & Technical Development Shimadzu(China)Co.Ltd.

hloramphenicol is an antibiotic and one of the potential contaminants in honey.Solid-phase extraction is the key pretreatment procedure for analysis of chloramphenicol in honey.In this work,an on-line pretreatment liquid chromatography-tandem mass spectrometer system for sensitive,reliable and higher throughput analysis was developed.With the methylcellulose-immobilized reversed-phase column,sugars in a honey sample were efficiently removed in 1 min.As a result,the limit of quantitation of chloramphenicol was 20 pg/mL（0.2 μg/kg honey）.

关键词： On-line pretreatment Liquid chromatography-mass spectrometry Chloramphenicol Honey

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Determination of Veterinary Drug Residues in Animal-derived Foods by Liquid chromatography-mass spectrometry

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Agricultural Biotechnology 2023年第1期12卷 84-86,93页

作者： Haowei CUI Kun XIN Guixia YANG Shandong China Quality Inspection Co. Ltd.Jining 272000China

[Objectives]This study was conducted to establish a rapid and effective method for simultaneous extraction of 54 kinds of veterinary drug residues in animal-derived food, including sulfonamides, quinolones, tetracyclines, malachite greens, penicillins, nitroimidazoles, tranquilizers and macrolides, by HPLC-MS. [Methods] The samples were extracted with 80% acetonitrile water(containing 0.1% formic acid), combined with QuEChERS extraction technology and C18 and PSA purification, analyzed by high performance Liquid chromatography-mass spectrometry, and quantified by external standard method. The target substances were analyzed on ZORBAX Eclipse C18 chromatographic column using 0.2% formic acid water and 0.2% methanol as mobile phases. The gradient elution mode was used for chromatographic separation and multiple reaction detection. [Results] In the linear range of 0.5-50.0 ng/ml, the linear relationship of the 54 kinds of veterinary drug residues was good, with correlation coefficients(r~2) greater than 0.995, and the detection limits ranged from 0.30 to 1.00 μg/kg. The results showed that the recovery ranged from 75.4% to 118.2% when different matrixes were added for recovery. [Conclusions] This method is simple, efficient, accurate, stable, and highly operable. It is applicable to simultaneous batch screening of veterinary drug residues in animal-derived food, and has high practical application value.

关键词： Animal-derived food Multiple veterinary drug residues Optimization Liquid chromatography-mass spectrometry

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Determination of Estrogens and Bisphenol A in Bovine Milk by Automated on-line C30 Solid-phase Extraction Coupled with High-performance Liquid chromatography-mass spectrometry

Determination of Estrogens and Bisphenol A in Bovine Milk by...

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第五届全国环境化学大会

作者： Wei Yan~1 Ying Li~1 Lixia Zhao~1 Jinming Lin~(1,2,*) (1 State Key Laboratory of Environmental Chemistry and Ecotoxicology,Research Center for Eco-Environmental Sciences,Chinese Academy of Sciences,P.O.Box 2871,Beijing 100085, China 2Department of Chemistry,Tsinghua University,Beijing 100084,China

Using triacontyl bonded silica(C) as on-line solid-phase extraction(SPE) material and a specially designed online analytical system which allowed large sample volume injection,a high speed and robust online SPE-HPLC-MS method was established for the analysis of five estrogens and bisphenol A(BPA) in milk samples.The milk sample is pretreated with acetonitrile for protein precipitation and then treated with primary

关键词： Triacontyl bonded silica Estrogens Liquid chromatography-mass spectrometry Spiked milk samples

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Quantification of perfluorinated compounds in atmospheric particulate shows potential connection with environmental event

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Journal of Environmental Sciences 2024年第2期136卷 237-247页

作者： Hua Tang Ying Wang Shengling Si Hongli Li David Da Yong Chen National Institute of Metrology 18 BeisanhuandongluChaoyang DistrictBeijing 100029China School of Chemistry and Materials Science Nanjing Normal UniversityNanjing 210023China Si Chuan Zhong Ce Biao Wu Technology Co.Ltd. Sichuan 610052China Department of Chemistry University of British ColumbiaVancouver V6T 1Z1BCCanada

A method of quantification of perfluorinated compounds(PFCs)from atmospheric particulate matter(APM)is described.A single step pretreatment method,selective pressurized liquid extraction(SPLE),was developed to reduce the high matrix background and avoid contamination from commonly used multiple sample pretreatment steps.An effective sorbent was selected to purify the PFCs during SPLE,followed by liquid chromatography-tandem mass spectrometry(LC–MS/MS),for quantification of PFCs.Conditions affecting the SPLE efficiency,including temperature,static extraction time,and number of extraction cycles used,were studied.The optimum conditions were found to be 120℃,10 min,and 3 cycles,respectively.LC-MS/MS method was developed to obtain the optimal sensitivity specific to PFCs.The method detection limits(MDLs)were 0.006 to 0.48 ng/g for the PFCs studied and the linear response range was from 0.1 to 100 ng/g.To ensure accurate values were obtained,each step of the experiment was evaluated and controlled to prevent contamination.The optimized method was tested by performing spiking experiments in natural particulate matter matrices and good rates of recovery and reproducibility were obtained for all target compounds.Finally,the method was successfully used to measure 16 PFCs in the APM samples collected in Beijing over five years from 2015 to 2019.It is observed that some PFCs follow the trend of total PFC changes,and can be attributed to the environment influencing events and policy enforcement,while others don't seem to change as much with time of the year or from year to year.

关键词： Selective pressurized liquid extraction Liquid chromatography-mass spectrometry Perfluorinated compounds Atmospheric particulate matter Pollution control

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Polarity-regulated derivatization-assisted LC-MS method for amino-containing metabolites profiling in gastric cancer

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Journal of Pharmaceutical Analysis 2023年第11期13卷 1353-1364页

作者： Jie Han Shilin Gong Xiqing Bian Yun Qian Guilan Wang Na Li Jian-Lin Wu State Key Laboratory of Quality Research in Chinese Medicine Macao Institute for Applied Research in Medicine and HealthMacao University of Science and TechnologyAvenida Wai LongTaipaMacao999078China Department of Gastroenterology and Hepatology Shenzhen University General HospitalShenzhenGuangdong518055China Department of Pediatrics Zhongshan Boai HospitalZhongshanGuangdong528403China

Amino-containing compounds,including amino acids,aliphatic amines,aromatic amines,small peptides and catecholamines,are involved in various biological processes and play vital roles in multiple metabolic pathways.Previous studies indicated that some amino-containing metabolites are significant diagnostic and prognostic biomarkers of gastric cancer.However,the discovery of precise biomarkers for the preoperative diagnosis of gastric cancer is still in an urgent need.Herein,we established a polarityregulated derivatization method coupled with Liquid chromatography-mass spectrometry(LC-MS)for amino-containing metabolites profiling in the serum samples of patients with gastric cancer and healthy controls,based on our newly designed and synthesized derivatization reagent(S)-3-(1-(diisopropoxyphosphoryl)pyrrolidine-2-carboxamido)-N-hydroxysuccinimidyl ester(3-DP-NHS).Enhanced separation efficiency and detection sensitivity for amino-containing metabolites were achieved after derivatization.This method exhibited good linearity,recovery,intra-and inter-day precision and accuracy.Only 5 mL serum is needed for untargeted analysis,enabling 202 amino-containing metabolites to be detected.Statistical analysis revealed altered amino acid metabolisms in patients with gastric cancer.Furthermore,ultra high performance liquid chromatography coupled with mass spectrometry(UHPLCMS/MS)analysis quantification revealed increased serum levels of tryptamine and decreased concentrations of arginine and tryptophan in patients with gastric cancer.Receiver operating characteristic(ROC)curves indicated that an increased tryptamine/tryptophan ratio could serve as a potential biomarker for gastric cancer diagnosis.This study demostrated the possibility of using serum amino acid biomarkers for gastric cancer diagnosis,providing new avenues for the treatment of gastric cancer.

关键词： Polarity-regulated derivatization Amino-containing metabolites Gastric cancer Liquid chromatography-mass spectrometry

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