RAPID COMMUNICATIONS IN MASS SPECTROMETRY
·
2017
·Vol. 32
·期 3
·262-268
·
IF 1.998
Xiafen Xu,Xinhui Li,Xianrui Liang
Rationale Metabolites of isoflavones have attracted much attention in recent years due to their potential bioactivities. However, the complex constituents of the metabolic system and the low level of metabolites make them difficult to analyze. A mass spectrometry (MS) method was applied in our identification of metabolites and study of their fragmentation pathways due to the advantages of rapidity, sensitivity, and low level of sample consumption. Methods Three isoflavone glycosides and their metabolites were identified using ultra-performance liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry (UPLC/QTOF-MS). These metabolites were obtained by anaerobically incubating three isoflavone glycosides with human intestinal flora. The characteristic fragments of isoflavone glycosides and their metabolites were used for the identification work. Results Two metabolites from ononin, three metabolites from irilone-4′- O -β-D-glucoside, and five metabolites from sissotrin were identified respectively by the retention time (RT), accurate mass, and mass spectral fragmentation patterns. The losses of the glucosyl group, CO from the [M+H] + ion were observed for all the three isoflavone glycosides. The characteristic retro-Diels-Alder (RDA) fragmentation patterns were used to differentiate the compounds. The metabolic pathways of the three isoflavone glycosides were proposed according to the identified chemical structures of the metabolites. Conclusions A selective, sensitive and rapid method was established for detecting and identifying three isoflavone glycosides and their metabolites using UPLC/QTOF-MS. The established method can be used for further rapid structural identification studies of metabolites and natural products. Furthermore, the proposed metabolic pathways will be helpful for understanding the in vivo metabolic process of isoflavone.
研究领域:
分析化学
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药理学
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营养学
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产品关联
DOI
PubMed
高影响因子
Toxins
·
2022
·Vol. 14
·期 2
·93
·
IF 5.075
Hongmei Liu,Zhihong Xuan,Jin Ye,Jinnan Chen,Meng Wang,Stephan Freitag,Rudolf Krska,Zehuan Liu,Li Li,Yu Wu,Songxue Wang
An immunoaffinity magnetic beads (IMBs) based automatic pretreatment method was developed for the quantitative analysis of deoxynivalenol (DON) by ultra-performance liquid chromatography and ultraviolet detector (UPLC-UV). First, N-hydroxysuccinimide-terminated magnetic beads (NHS-MBs) with good magnetic responsivity and dispersibility were synthesized and characterized by optical microscopy, scanning electron microscopy (SEM), and laser diffraction-based particle size analyzer. Then, the amino groups of anti-DON monoclonal antibody (mAb) and the NHS groups of NHS-MBs were linked by covalent bonds to prepare IMB, without any activation reagent. The essential factors affecting the binding and elution of DON were meticulously tuned. Under optimal conditions, DON could be extracted from a real sample and eluted from IMB by water, enabling environmentally friendly and green analysis. Hence, there was no need for dilution or evaporation prior to UPLC-UV analysis. DON in 20 samples could be purified and concentrated within 30 min by the mycotoxin automated purification instrument (MAPI), allowing for automated, green, high-throughput and simple clean-up. Recoveries at four distinct spiking levels in corn and wheat ranged from 92.0% to 109.5% with good relative standard deviations (RSD, 2.1–7.0%). Comparing the test results of IAC and IMB in commercial samples demonstrated the reliability and superiority of IMB for quantitatively analyzing massive samples.Keywords:deoxynivalenol;immunoaffinity magnetic beads;automatic;UPLC-UVKey Contribution:An immunoaffinity magnetic beads-based automatic pretreatment method was developed for the quantitative analysis of deoxynivalenol by UPLC-UV, with water used as the solvent for extraction and elution.
研究领域:
分析化学
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毒理学
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食品科学
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DOI
PubMed
高影响因子
FITOTERAPIA
·
2025
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IF 2.6
Wenyuan Li,Lin Chen,Minpeng Li,Kaiye Peng,Xuemei Lin,Yifan Feng,Yun Zou,Xia Wu
In this study, the chemical constituents of branch bark and root bark of Morus alba L. were first qualitatively analyzed by UPLC-Q/TOF-MS. A total of 40 compounds were identified, including 20 flavonoids, 3 stilbenes, 1 phenolic acid, 1 alkaloid, 5 arylbenzofurans and 10 Diels-Alder adducts. Of these, 19 compounds were specific to the root bark, 10 to the branch bark, and 11 were common to both. Total phenolic and flavonoid contents were determined, and anti-inflammatory activities were evaluated. Ethyl acetate extracts of both significantly inhibited NO secretion, with the root bark showing a stronger effect than the branch bark. Chemical components of branch bark were further separated, and the anti-inflammatory activities of these isolated compounds were investigated. Eight compounds were isolated from the ethyl acetate extract of the branch bark of Morus alba L. . These compounds were able to inhibit the release of inflammatory factors, including NO, IL-6, and IL-1β, in a concentration-dependent manner. Among them, compounds SZP-1, SZP-6 and SZP-8 exhibited superior in vitro anti-inflammatory activity, comparable to the positive drug meloxicam at high concentrations. In addition, the quality standard of the branch bark of Morus alba L. was established for the first time according to the 2020 edition of the Chinese Pharmacopoeia. This study provides valuable insights into the medicinal value of the branch bark of Morus alba L. and promotes the comprehensive utilization of mulberry branch resources.
研究领域:
药理学
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植物化学
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分析化学
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DOI
PubMed
高影响因子
MOLECULES
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2018
·Vol. 23
·期 2
·459
·
IF 3.098
Ya Song,Xiao-Qun Wei,Mei-Ying Li,Xue-Wu Duan,Yuan-Ming Sun,Rui-Li Yang,Xiang-Dong Su,Ri-Ming Huang,Hong Wang
The aim of this work was to evaluate the main nutrients and their antioxidant properties of a Chinese wild edible fruit,Passiflora foetida,collected from the ecoregion of Hainan province, China. The analytical results revealed thatP. foetidafruits were rich in amino acids (1097 mg/100 g in total), minerals (595.75 mg/100 g in total), and unsaturated fatty acids (74.18 g/100 g in total fat). The lyophilized powder of edible portion contained the higher polyphenols content than the inedible portion powder. The UPLC-Q-TOF-MSEanalysis of the extractable and non-extractable phenolics indicated the presence of 65 compounds including 39 free phenolics, 14 insoluble-glycoside-phenolics, and 22 insoluble-ester-phenolics. In addition, the non-extractable phenolics obtained by alkali hydrolysis showed significant antioxidant activities by/through DPPH and ABTS radical scavenging. These findings ofP. foetidafruits, for the first time, suggest that these polyphenol-rich fruits may have potential nutraceutical efficacies.Keywords:Passiflora foetida;fruit;nutritional composition;antioxidant properties;UPLC-MS;phenolic compound
研究领域:
营养学
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植物化学
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食品科学
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产品关联
DOI
PubMed
高影响因子
Foods
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2023
·Vol. 12
·期 24
·4434
·
IF 5.2
Ya-bo Ba,Rui Li,Jia-yi Zhang,Liang Zou,Ding-Tao Wu,Yi-chen Hu
Although quinoa is nutritious, its high fat content and lipase activity make it easily oxidized during storage. Meanwhile, quinoa’s lipid composition and changes during storage are still unknown. Therefore, we stored fresh quinoa flour at low temperature and low humidity (LL), normal temperature and normal humidity (NN), and high temperature and high humidity (HH) conditions for 120 days to assess its oxidative stability and to monitor the changes in lipid composition. Herein, the contents of fatty acids, the peroxide values, the malondialdehyde values, and the lipase activity in quinoa flour during storage are determined to evaluate its oxidation stability. At LL and NN conditions, the contents of fatty acids, the peroxide values, the malondialdehyde values, and the lipase activity changed slowly. They were 3 (LL) and 5 times (NN), 2.7 (LL) and 4.7 times (NN), 1.4 (LL) and 2.3 times (NN), and 1.5 (LL) and 1.6 times (NN) the initial content at storage up to 120 d. However, with the prolongation of storage time under HH conditions, they all increased significantly to 8, 6.6, 3, and 2 times the original content. Moreover, during the storage of quinoa under LL, NN, and HH conditions for 120 days, we continuously monitored the lipid composition of quinoa grains with UPLC-Q-Exactive Orbitrap MS/MS. We identified a total of 14 subclasses of 229 lipids, including 90 significantly different lipid species. PCA and PLS-DA showed that quinoa lipids in HH conditions changed significantly with prolonged storage; among these, the TG and DG classes were the most susceptible to oxidation, which could distinguish fresh quinoa from oxidized quinoa. Simultaneously, we also found that lipase activity has a significant impact on lipid metabolism through correlation analysis, which also indicates that enzyme inactivation treatment can slow down lipid hydrolysis and oxidation during storage. To explore the mechanism of these changes, we also identified twelve important lipid metabolism pathways during quinoa storage. In conclusion, our study advances knowledge of the storage stability and lipid oxidation mechanisms of quinoa and provides a theoretical basis for setting the shelf life of quinoa.Keywords:quinoa flour;lipase;storage oxidation;lipidomics;UPLC-Q-Exactive Orbitrap Mass spectrometry
研究领域:
食品科学
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植物学
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代谢组学
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产品关联
DOI
PubMed
高影响因子
INTERNATIONAL JOURNAL OF BIOLOGICAL MACROMOLECULES
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2024
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IF 7.7
Yanyun Zhu,Yunyun Zheng,Bingge Liu,Kouadio Jean Eric-Parfait Kouame,Ebenezer O. Falade,Jianchu Chen,Xingqian Ye
Monosaccharide composition and glycosidic linkages analysis are essential for the structural characterization and biological activity research of polysaccharides. To simplify the analysis steps and improve detection efficiency, this study developed monosaccharide compositions and glycosidic linkages detection methods based on UPLC-QqQ-MS/MS, and established a plant polysaccharide glycosidic linkages library. Furthermore, the detailed analysis process of monosaccharide compositions and glycosidic linkages was presented through a plant polysaccharide (Chinese bayberry wine polysaccharide, CPW) example. The results showed that the monosaccharide analysis method could identify and quantify 20 monosaccharides within 13 min by 6 chromatograms. By this method, 7 monosaccharides were detected in CPW, which was consistent with previous results obtained using ion chromatography. Meanwhile, the UPLC-QqQ-MS/MS based method could analyze 112 glycosidic linkages of 9 plant monosaccharides within 30 min, and the results were distributed on 11 chromatograms. According to the approach, 44 different glycosidic linkages were identified in CPW. Based on Congo red assay and molecular weight as well as our findings of monosaccharide composition and glycosidic linkages, we proposed that CPW may consist of two distinct sugar chains: One composed of 1–2,4-Rha, 1–3,4-GalA, and 1-F-Ara, and the other composed of 1–3,4-Gal, 1–4-Gal, 1–3,4,6-Gal, and 1-F-Ara.
研究领域:
分析化学
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植物学
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生物化学
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产品关联
DOI
PubMed
高影响因子
ACS ES&T Water
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2024
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IF 4.8
Jian Pan,Qizheng Zhuo,Xi-Zhi Niu,Yaxiong Zeng,Haiqiang Wang,Baohong Guan
Trace pharmaceutical active compounds (PhACs) in drinking water have been attracting wide attention due to their hazardous impacts and negative effects on human health and ecology, and their removal from drinking water has been becoming a priority. Here, we used the methods of UPLC-triple-TOF/MS to screen PhACs in the Shangxi Drinking Water Treatment Plant (DWTP) in Zhejiang, East China, and found the occurrence of ibuprofen, propranolol, and gemfibrozil. The current processes of DWTP cannot remove PhACs effectively. Gemfibrozil has the highest average concentrations among PhACs with 0.464, 1.292, and 0.583 ng/L at the units of sand filtration, ozonation-biological aerated filter (ozonation-BAF), and clean water pool, respectively. In a pilot-scale test, the ozonation removes 21.1–67.9% of gemfibrozil, while the catalytic ozonation with ceramic catalyst achieves removal efficiencies of 55.6–85.2% in 3.6 min. Gemfibrozil is degraded by catalytic ozonation through two pathways: initiated by ·OH reaction with aromatic ring C2 or started with ·OH attacking aromatic ring C3. This study reveals the existence of PhACs in DWTP and validates a feasible way of catalytic ozonation with a ceramic catalyst to remove them quickly.
研究领域:
环境科学
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公共卫生
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分析化学
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产品关联
DOI
高影响因子
INTERNATIONAL JOURNAL OF BIOLOGICAL MACROMOLECULES
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2024
·
IF 7.7
Xiao-Jun Li,Shi-Jun Xiao,Yi Heng Xie,Jiang Chen,Hai-Rong Xu,Yuan Yin,Rui Zhang,Tong Yang,Tong-Yu Zhou,Si-Yan Zhang,Pei Hu,Li-Ming Gao,Hui-Ping Peng
An innovative acidic hydrolysate fingerprinting workflow was proposed for the characterization of Lyophyllum Decastes polysaccharide (LDP) by ultra performance liquid chromatography-mass spectrometry (UPLC-MS). The crude polysaccharides were firstly separated and purified by using DE-52 column and the BRT GPC purification system, respectively. The molecular weight and monosaccharide content of homogeneous polysaccharides were ascertained by utilizing HPGPC and ion chromatography separately. Secondly, the linkage of LDP was identified by methylation analysis and 1D/2D NMR spectra. The UPLC-MS/MS was used to scan and identify the acidic hydrolysate products of LDP using the PGC column. The oligosaccharides were collected by chromatography and identified by mass spectrometry. Thirdly, the expression of IL-1β, IL-6, iNOS, TNF-α and IFNAR-I was measured in order to assess the immunological activity of LDP. Besides, the targeted receptors identification of polysaccharides was performed by screening the expression of TLRs family protein. The results showed that oligosaccharide fragments with different molecular weights can be obtained by partial hydrolysis, which further verified that the structures of LDP polysaccharides was a 1–6-linked β-glucan. Moreover, the LDP polysaccharide can up-regulate the content of IL-1β, IL-6, iNOS, TNF-α and IFNAR-I and plays an important immunoregulation role through TLRs family.
研究领域:
生物化学
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免疫学
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产品关联
DOI
PubMed
高影响因子
INDUSTRIAL CROPS AND PRODUCTS
·
2020
·
IF 4.244
Meng Pan,Qicheng Lei,Hong Zhang
Screening of active ingredients in plants is critical for the development of medicinal plants. As a traditional medicinal material, Eucalyptus globulus Labill leaves are regarded as a potential raw material that can be developed as a pesticide because of its original activity. This study proposes a molecular docking assisted UPLC-MS/MS, GC–MS/MS method for the identification and prediction of insecticidal ingredients in the extracts of Eucalyptus globulus leaves. The extracts of Eucalyptus globulus leaves were analyzed by UPLC-MS/MS, GC–MS/MS, 34 aqueous ingredients and 35 volatile ingredients were identified. The identified ingredients were docked with repellent receptor (2KSL). The results showed that protocatechuic acid had strong 2KSL inhibitory activity, which was presumed to be the main reason for the inhibition of 2KSL. Finally, the antifeedant experiment of protocatechuic acid on Henosepilachna vigintioctopunctata (Fabricius) was carried out. The results indicate that the method can effectively screen the active ingredients from the medicinal plants.
研究领域:
植物学
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药理学
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昆虫学
✓ 已验证
产品关联
DOI
高影响因子
Foods
·
2023
·Vol. 12
·期 15
·2875
·
IF 5.2
Yibo Dong,Xiaolong Yao,Wanping Zhang,Xiaomao Wu
3,4-dichloroaniline (3,4-DCA) and 3,5-dichloroaniline (3,5-DCA) are, respectively, the primary metabolites deriving from the breakdown of phenylurea herbicides and dicarboximide fungicides in both soils and plants, whose residues in vegetable products have a heightened concern considering their higher health risks to humans and greater toxicity than the parent compounds in the environment. In this study, a sensitive high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was developed for the simultaneous determination of 3,4-DCA and 3,5-DCA residues in chive products based on the optimization of HPLC-MS/MS chromatographic and mass-spectrometric conditions using the standard substances and the modified QuEChERS preparation technique. The preparation efficiency of 3,4-DCA and 3,5-DCA from chive samples showed that acetonitrile was the best extractant. The combination of the purification agent graphite carbon black + primary secondary amine and the eluting agent acetonitrile + toluene (4:1,v/v) had a satisfactory purification effect. The linear correlation coefficients (R2) were more than 0.996 with the six concentration range of 0.001–1.000 mg/L for 3,4-DCA and 3,5-DCA. The limit of detection and limit of quantitation of this method was 0.6 and 2.0 µg/kg for 3,4-DCA, as well as 1.0 and 3.0 µg/kg for 3,5-DCA, respectively. The matrix effect range of 3,4-DCA and 3,5-DCA in chive tissues was from −9.0% to −2.6% and from −4.4% to 2.3%, respectively. The fortified recovery of 3,4-DCA and 3,5-DCA in chive samples at four spiked levels of 0.001–1.000 mg/kg was 75.3–86.0% and 78.2–98.1%, with the relative standard deviation of 2.1–8.5% and 1.4–11.9%, respectively. The limit of detection (LOD) and limit of quantification (LOQ) of the method were 0.6, 2.0, and 1.0, 3.03 for 4-DCA and 3,5-DCA, respectively. This study highlights that the analytical method established here can efficiently and sensitively detect residues of 3,4-DCA and 3,5-DCA residues for monitoring chive products. The method was successfully applied to 60 batches of actual vegetable samples from different regions.Keywords:3,4-dichloroaniline;3,5-dichloroaniline;simultaneous determination;UPLC-MS/MS;chive
研究领域:
分析化学
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食品安全
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环境科学
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF MASS SPECTROMETRY
·
2021
·Vol. 57
·期 1
·e4795
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IF 1.982
Lili Song,Hongqing Yin,Rui Han,Jingfang Li,Ningning Ma,Yan Wang,Hong Guo
Du Zhong Formula (DZF), a traditional Chinese medicine formula derived from BeiJiQianJinYaoFang, is used to treat kidney deficiency and lumbago. In this study, ultra-high-performance liquid chromatography quadrupole time-of-flight mass spectrometer (UPLC-Q-TOF/MS) technique combined with pattern recognition analysis was applied for analysis of metabolic profiles of the bioactive components of the DZF in rat biological samples. In this experiment, a total of 73 compounds, including 53 prototype components and 20 metabolites, were identified tentatively in vivo compared with blank urine, plasma, feces, and cerebrospinal fluid (CSF). The prototype ingredients in DZF include terpenoids, gingerols, phenylpropanoids, alkaloids, phenanthrenes, bibenzyls, organic acids, and other ingredients. The metabolic pathways of DZF involved reduction, demethylation, hydroxylation, desugarization, deoxygenation, glucuronidation, sulfation, and methylation. The proposed method could develop an integrated template approach to analyze screening and identification of the bioactive components in plasma, urine, feces, and CSF after oral administration of herb medicines. Additionally, this investigation might provide helpful chemical information for further pharmacology and activity mechanism of DZF.
研究领域:
药理学
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中医药
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分析化学
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代谢组学
✓ 已验证
DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
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2026
·
IF 2.5
Peiqi Sun,Fei Hang,Jiayang Wang,Yuanye Jiang,Lingyun Pan,Cheng Hu
Sphingosine (SP), dihydro-sphingosine (DSP), and sphingosine 1-phosphate (S1P) are integral metabolites in the sphingolipid pathway. They exhibit intricate and diverse functions in the development of metabolic-associated fatty liver disease (MAFLD). In this study, we developed a highly sensitive and specific analytical approach for the concurrent quantification of these three sphingolipids in human plasma, utilizing ultra-high-performance liquid chromatography (UPLC), in conjunction with tandem mass spectrometry (MS/MS). A stripped biological matrix was generated through optimized activated‑carbon treatment to facilitate more accurate calibration. The sample preparation involved a straightforward protein precipitation method using methanol, followed by concentrating the supernatant and reconstituting it prior to injection. Detection was executed in the multiple reaction monitoring mode with a triple quadrupole mass spectrometer. The chromatographic separation was achieved on a Waters ACQUITY UPLC HSS C 18 column employing gradient elution. D-erythro-sphingosine-d 7 served as the internal standard. The newly established method conformed to recognized standards for selectivity, linearity, accuracy, precision, recovery, matrix effects, and stability. This technique was effectively applied to quantify the three sphingolipid metabolites in plasma samples collected from patients diagnosed with MAFLD ( n = 30), and healthy controls (n = 30). Analysis of the data revealed significant differences between the groups, with the levels of SP, DSP, and S1P considerably elevated in MAFLD patients compared to healthy subjects.
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产品关联
DOI
高影响因子
危险品化学品经营许可证（带存储）