Foods
·
2023
·Vol. 12
·期 16
·3123
·
IF 5.2
Xiaolei Fang,Yanping Chen,Jie Gao,Zimu Run,He Chen,Ruoqi Shi,Yingqiu Li,Haihua Zhang,Yuan Liu
The volatiles in coffee play an important part in the overall flavor profile. In this study, GC–TOF/MS and GC×GC–TOF/MS were used to detect the volatile organic compounds (VOCs) in coffee samples of three different brands at three states (bean, powder, and brew). The differences between the two methods in characterizing VOCs were analyzed using the Venn diagram and PCA (principal component analysis). The important aroma-contributing compounds were further compared and analyzed. The results of the venn diagrams of different coffee samples showed that most VOCs existed in 2–3 kinds of coffee. The PCA of VOCs in different coffee samples showed that the VOCs detected by GC–TOF/MS could distinguish the coffee samples in the different states. GC×GC–TOF/MS was suitable for the further identification and differentiation of the different brands of coffee samples. In addition, pyridine, pyrrole, alcohols, and phenols greatly contributed to distinguishing coffee in three states, and alcohols greatly contributed to distinguishing the three brands of coffee.Keywords:coffee;GC×GC–TOF/MS;GC–TOF/MS;volatile organic components
研究领域:
食品科学
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分析化学
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产品关联
DOI
PubMed
高影响因子
FOOD CHEMISTRY
·
2025
·
IF 9.8
Zhang-Na Qin,Jia-Min Chen,Jia-Wei Li,Zhen-Peng Zhen,Qi-Zhao Chen,Zhi-Qiang Zhang,Gui-Hua Wang,Yu-Feng Gao
The slight structural differences between carbohydrate isomers pose considerable difficulties for their identification and quantification. Herein, a rapid method for the absolute quantification of glucose and fructose isomers using matrix-assisted laser desorption/ionization time-of-flight/time-of-flight tandem mass spectrometry (MALDI-TOF/TOF MS/MS). A novel reagent, 4-trimethylamino-6-(4-methoxy-1-naphthyl)-1,3,5-triazine-2-(3-aminophenylboronic acid) (TMNTA), was synthesized and employed as a reactive matrix. This matrix significantly enhances the ionization efficiency of monosaccharides while avoiding matrix interferences. Glucose- 13 C 6 was utilized as an internal standard for the quantitative analysis of both monosaccharides, exhibiting a strong linear correlation (R 2 ≥ 0.990). By integrating the concentration relationships of glucose and fructose derived from two diagnostic ions produced from the TMNTA-derivatized monosaccharides, this approach facilitates the absolute quantification of glucose and fructose. The method was successfully applied to the absolute quantification of these monosaccharides in honey. The proposed approach offers a simple, rapid, and high-throughput analysis of glucose and fructose isomers in complex samples.
研究领域:
分析化学
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食品科学
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生物化学
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DOI
PubMed
高影响因子
Journal of Pharmaceutical Analysis
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2017
·
IF 0
Min Liu,Yan Cao,Diya Lv,Wen Zhang,Zhenyu Zhu,Hai Zhang,Yifeng Chai
According to the Chinese Pharmacopoeia 2015, only processed Aconitum tubers can be clinically applied, and the effect of processing is unclear. This research aimed to explore the effect of processing on cardiac efficacy of alkaloids in Aconitum tubers. First, the chemical ingredients in unprocessed and processed Aconitum tubers were identified and compared by using high performance liquid chromatography time-of-flight mass spectrometry (HPLC-TOF/MS) and multivariate pattern recognition methods. Then the representative alkaloids in Aconitum tubers, aconitine, benzoylaconine, and aconine, which belong to diester-diterpenoid alkaloids, monoester-diterpenoid alkaloids, and amine-diterpenoid alkaloids, respectively, were selected for further validation of attenuated mechanism. Subsequent pharmacological experiments with aconitine, benzoylaconine, and aconine in SD rats were used for validate the effect of processing on cardiac functions. After processing the Aconitum tubers, it was found that the contents of diester-diterpenoid alkaloids were reduced, and those of monoester-diterpenoid alkaloids and amine-diterpenoid alkaloids were increased, suggesting that diester-diterpenoid alkaloids were transformed into monoester-diterpenoid alkaloids and amine-diterpenoid alkaloids. Through further decocting the aconitine in boiling water, it was confirmed that the three alkaloids could be progressively transformed. Pharmacological experiments with aconitine, benzoylaconine, and aconine in SD rats showed that aconitine at a dose of 0.01 mg/kg and aconine at a dose of 10 mg/kg enhanced the cardiac function, while benzoylaconine at a dose of 2 mg/kg weakened the cardiac function. The effect of processing is attributed to the transformation of the most toxic diester-diterpenoid alkaloids into less toxic monoester-diterpenoid alkaloids and amine-diterpenoid alkaloids.
研究领域:
中药学
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药理学
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DOI
PubMed
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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2025
·
IF 3.1
Zhao-liang Hu,Wen-yu Zou,Peng-wei Hu,Ke-ran Chen,Jia-ying Liu,Jie Deng,Ju-cui Yang,Min Song,Yu-ting Lu,Tai-jun Hang
Letrozole, a nonsteroidal aromatase inhibitor of the triazole class, is widely used in breast cancer treatment. Its quality and stability directly influence therapeutic efficacy and safety. However, systematic characterization of its related substances (RSs) remains insufficiently documented. In this study, letrozole RSs were separated by an established HPLC-UV method and identified with LC-Q-TOF/MS determination following the ICH Q1A(R2) guidelines. 27 RSs were detected, including 11 process-related impurities and 16 previously unreported degradation products. Structural elucidation and degradation pathway analysis were performed for all the RSs by using their chromatographic retention behaviors, DAD spectral features, and high-resolution mass spectrometric data. Three main degradation pathways were proposed for them, including substitution on the triazole ring, hydrolysis of the cyano groups, and oxidation of the benzyl moiety. Furthermore, to support impurity risk assessment, the genotoxicities of all the RSs were evaluated using in-silico models according to the ICH M7 (R2) guideline. Most of the RSs were evaluated to be non-mutagenic, however four of them were identified as structurally alerting. These findings contribute to a better understanding of the stability behavior of letrozole and provide a scientific basis for the drug quality risk management from its related substances test and control point of view.
研究领域:
药物化学
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分析化学
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药学
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DOI
PubMed
高影响因子
MOLECULES
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2020
·Vol. 25
·期 5
·1082
·
IF 3.267
Limin Li,Bin Hao,Yulong Zhang,Shen Ji,Guixin Chou
Militarine, a natural glucosyloxybenzyl 2-isobutylmalate, isolated fromBletilla striata, was reported with a prominent neuroprotective effect recently. The limited information on the metabolism of militarine impedes comprehension of its biological actions and pharmacology. This study aimed to investigate the metabolite profile and the distribution of militarine in vivo, which help to clarify the action mechanism further. A total of 71 metabolites (57 new metabolites) in rats were identified with a systematic method by ultra-high-performance liquid chromatography combined with quadrupole time-of-flight tandem mass spectrometry (UPLC-Q-TOF-MS/MS). The proposed metabolic pathways of militarine include hydrolyzation, oxidation, glycosylation, esterification, sulfation, glucuronidation and glycine conjugation. Militarine and its metabolites were distributed extensively in the treated rats. Notably, six metabolites of militarine were identified in cerebrospinal fluid (CSF), which were highly consistent with the metabolites after oral administration of gastrodin in rats. Among the metabolites in CSF, five of them were not reported before. It is the first systematic metabolic study of militarine in vivo, which is very helpful for better comprehension of the functions and the central nervous system (CNS) bioactivities of militarine. The findings will also provide an essential reference for the metabolism of other glucosylated benzyl esters of succinic, malic, tartaric and citric acids.Keywords:militarine;metabolite identification;metabolic profiles;UPLC-Q-TOF-MS/MS
研究领域:
药理学
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分析化学
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产品关联
DOI
PubMed
高影响因子
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
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2023
·Vol. 415
·期 23
·5575-5588
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IF 4.3
Liu Yuanyuan,Han Yutong,Zhu Wenjie,Luo Qingming,Yuan Jing,Liu Xin
Glycosylation is one of the most common types of post-translational modifications in mammals. It is well known that N-glycans play a key role in cell adhesion, differentiation, synapsis, and myelination during the development of the mammalian central nervous system (CNS). Neuropathological symptoms (such as epilepsy and Alzheimer’s disease) are usually accompanied by N-glycosylation changes. In this study, we extracted N-glycan chains from eight regions of the mouse brain, and combined high-throughput, high-resolution matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF/MS) with the Fmoc N-hydroxysuccinimide ester (Fmoc-OSU) derivatization method to improve the sensitivity of glycan detection to characterize the total N-glycans in the mouse brain. A total of 96 N-glycan moieties were detected. An exhaustive examination of the relative abundance of N-glycans, coupled with a comparative analysis of differences, has uncovered discernible variations of statistical significance, including high mannose, fucosylated, sialylated, and galactosylated N-glycans. According to our investigations, a thorough and regionally specific cartography of glycans within the brain can facilitate the investigation of glycan-mediated mechanisms related to both the developmental trajectory and functional output of the brain. Additionally, this approach may serve as a basis for identifying potential biomarkers that are relevant to various brain-associated pathologies. Graphical Abstract
研究领域:
生物化学
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神经科学
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分子生物学
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产品关联
DOI
PubMed
高影响因子
Frontiers in Chemistry
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2022
·
IF 5.545
Liu Qian-Bao,Lu Jing-Guang,Jiang Zhi-Hong,Zhang Wei,Li Wen-Jia,Qian Zheng-Ming,Bai Li-Ping
Time-of-flight secondary ion mass spectrometry (TOF-SIMS) is a sensitive surface analytical technology, which can simultaneously acquire diverse chemical components and their precise locations on the surfaces of samples without any requirements for chemical damage pretreatments or additional matrices. Commonly, the quality control of TCMs (traditional Chinese medicines) is limited by the qualitative and quantitative evaluations of the specifically extractive constituents. In this study, a practical sample preparation strategy named two-layered media embedding sample preparation was developed to obtain ideal freezing sections of dried materials of Cordyceps sinensis. Meanwhile, the well-established sample preparation method was applied for in situ chemical profiling and imaging of natural (NCS) and cultured Cordyceps sinensis (CCS) by using TOF-SIMS. More than 200 components were tentatively identified and imaged in NCS and CCS at the same time. Mass spectrometry imaging revealed that most components have even distributions in caterpillars of Cordyceps sinensis, while TAGs, DAGs, MAGs, and FAs only have distributions outside caterpillars’ digestive chambers. This is the first time that components were in situ imaged for Cordyceps sinensis to exhibit the chemical distributions which have never been achieved by other analytical techniques so far. In addition, chemometrics was used to simplify and explain the massive TOF-SIMS mass data sets, which revealed the high chemical similarity between CCS and NCS. Furthermore, the relative quantification of TOF-SIMS data showed that CCS has comparable proportions of amino acids, nucleosides, monosaccharides, sphingolipids, sterols and other principles to NCS except for fatty acids, glycerides and glycerophospholipids. The higher amounts of TAGs and DAGs in CCS were confirmed by quantitative 1H-NMR, indicating reliable relative quantification of TOF-SIMS. In general, our research developed a novel approach of TOF-SIMS for in situ chemical analysis of TCMs, and its successful application in comparative study of CCS and NCS suggested that TOF-SIMS is an advanced and promising analytical technology for the research of TCMs.
研究领域:
分析化学
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中药学
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生物化学
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DOI
PubMed
高影响因子
Chemistry Central Journal
·
2017
·Vol. 11
·期 1
·1-15
·
IF 2.442
Zhang Xiaoyan,Sun Wenbo,Yang Zhou,Liang Yan,Zhou Wei,Tang Lei
Background
Toddalia asiatica root bark as an effective hemostatic natural medicine or Chinese materia medica was applied in China for long history, its complex drug action mechanisms and unclear substance basis have been constraining the development of this drug.Results An intelligentized strategy by LC-ESI Q-TOF MSE was presented in this study for rapid identification of hemostatic chemical constituents from this natural medicine. Chromatographic separation was performed on a C18 column (150 mm × 2.1 mm, 1.8 μm), the MSE data in both negative and positive ion modes were acquired to record the high-accuracy MS and MS/MS data of all precursor ions. To reduce the false positive identifications, structural confirmation was conducted by comparison with the isolated reference standards (tR and MS, MS/MS data) or matching with natural product databases. Bioassay-guided fractionation of the extract of T. asiatica root bark was also carried out.Conclusion sAs a consequence, 31 natural compounds in T. asiatica root bark got putatively characterized. There were four main coumarins, isopimpinellin (Cp.23), pimpinellin (Cp.24), coumurrayin (Cp.30) and phellopterin (Cp.34) isolated and identified from T. asiatica root bark. The present study provided candidate strategy that helps to effectively identify the primary natural compounds of TCM or other complex natural medicines, and then promote development and application of natural medicines and their medicinal resources.
研究领域:
药理学
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中药学
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分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2022
·
IF 3.571
Jing Jiang,Zhao-liang Hu,Hamza Boucetta,Jia-ming Liu,Min Song,Tai-jun Hang,Yu-ting Lu
Flumazenil is an imidazobenzodiazepine derivative that antagonizes the actions of benzodiazepines . The degradation pathway elucidation plays an important role in the drug quality control. In this work, a reliable LC-Q-TOF/MS method was developed to separate and identify the degradation products of flumazenil generated in the stress testing conducted according to the ICH Q1A(R2) guideline. Fifteen degradation products were detected in total including three reported impurities and twelve unknown impurities. Based on the chromatographic and mass spectrometric data acquired, the structures of all the degradation products were identified. Besides, two major degradants were synthetized and further confirmed by NMR. The degradation pathways of flumazenil were elucidated, and the degradation characteristics of benzodiazepines were also discussed. The obtained results are of both great importance for the quality control of flumazenil and good reference for the degradation study of other benzodiazepines.
研究领域:
药物化学
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分析化学
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药学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
FOOD CHEMISTRY
·
2022
·
IF 9.231
Qingwen Huang,Wenbo Guo,Xiuying Zhao,Haojie Cao,Kai Fan,Jiajia Meng,Dongxia Nie,Yongjiang Wu,Zheng Han
Due to the challenge of hundreds of potential mycotoxins that may be present in cereals, a rapid and reliable ultra-high performance liquid chromatography coupled with quadrupole-time-of-flight tandem mass spectrometry (UHPLC-Q-TOF MS) technique was developed for universal screening of 200 mycotoxins (prototype, emerging and related derivatives) in cereals. With satisfactory sensitivity of accurate mass full-spectrum acquisition, it is feasible to preliminarily identify tentative untargeted mycotoxins with a large range of polarity without reference materials. The current screening method was also validated by the determination of 33 typical mycotoxins, and the screening detection limits in the range of 0.5–100 μg kg −1 were established in cereals. In total, 138 stored samples were contaminated by 46 mycotoxins and their metabolites, some of which were firstly reported in cereals, posing emerging potential health risks to humans and animals. Furthermore, the accumulation, transformation and degradation mechanisms of typical mycotoxins in cereals were investigated under real storage conditions.
研究领域:
食品安全
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分析化学
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毒理学
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产品关联
DOI
PubMed
高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2012
·Vol. 27
·期 4
·509-514
·
IF 1.966
Linling Lu,Dawei Qian,Jing Yang,Shu Jiang,Jianming Guo,Er-xin Shang,Jin-ao Duan
In this paper, ultraperformance liquid chromatography/quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF/MS) and the MetaboLynx™ software combined with mass defect filtering were applied to identity the metabolites of isoquercitrin using an intestinal mixture of bacteria and 96 isolated strains from human feces. The human incubated samples collected for 72 h in the anaerobic incubator and extracted with ethyl acetate were analyzed by UPLC-Q-TOF/MS within 10 min. The parent compound and five metabolites were identified by eight isolated strains, including Bacillus sp. 17, Veillonella sp. 23 and 32 and Bacteroides sp. 40, 41, 56, 75 and 88 in vitro . The results indicate that quercetin, acetylated isoquercitrin, dehydroxylated isoquercitrin, hydroxylated quercetin and hydroxymethylated quercetin are the major metabolites of isoquercitrin. Furthermore, a possible metabolic pathway for the biotransformation of isoquercitrin was established in intestinal flora. This study will be helpful for understanding the metabolic route of isoquercitrin and the role of different intestinal bacteria in the metabolism of natural compounds. Copyright © 2012 John Wiley & Sons, Ltd.
研究领域:
分析化学
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微生物学
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代谢组学
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产品关联
DOI
PubMed
高影响因子
Forensic Toxicology
·
2016
·Vol. 34
·期 2
·398-402
·
IF 0
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
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分析化学
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毒理学
✓ 已验证
DOI
PubMed
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