BIOMEDICAL CHROMATOGRAPHY
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2020
·Vol. 35
·期 3
·e4991
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IF 1.728
Li-Juan Nie,Jun Liang,Feng Shan,Ya-Yun Xu,Chun-Yu Yan,Xuan Zhou,Zhuo-Yu Cheng,Qing-Rong Xia
A simple, rapid, and selective ultra-performance liquid chromatography–tandem mass spectrometry method for determination of l -carnitine (LC) and acetyl- l- carnitine (ALC) in human serum was developed. Acetyl- l- carnitine-d 3 (ALC-d 3 ) was selected as internal standard (IS). After protein precipitation with acetonitrile–water (1 mL, 2:1, v/v), the analytes and IS were separated on a 2.5-μm XSelect HSS T3 C 18 column by gradient elution with methanol–water (containing 0.01% ammonia water) as the mobile phase at a flow rate of 0.2 mL/min. Analytes were detected with multiple reaction monitoring using a positive scan mode with electrospray ionization. Good linearity ( R 2 > 0.999) was observed in the concentration range for LC and ALC. The inter- and intra-day values of relative error were −10.4% to 10.0% with CVs less than 9.84%. The average recoveries of the two analytes were 91.29%–98.23%. Blood samples containing LC and ALC were stable under various storage conditions. Normal, haemolytic, and hyperlipidaemic serum had no significant effect on the quantification of LC and ALC. This method was successfully applied to study the concentrations of endogenous LC and ALC in the serum of patients with first-episode depression.
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JOURNAL OF ETHNOPHARMACOLOGY
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2019
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IF 3.414
Xia Gao,Chaojie Huang,Ting Geng,Xialin Chen,Jiajia Wang,Jingying Liu,Kun Duan,Liang Cao,Zhenzhong Wang,Wei Xiao
Ethnopharmacological relevance Reduning injection (RDN), a patented traditional Chinese medicine , has the obvious antipyretic effect and has been widely used in China. Although some previous studies proved its antipyretic effect by animal efficacy experiment or clinical observation, its holistic mechanism in vivo was still unclear. Aim of the study To comprehensively elucidate the antipyretic mechanism of RDN, the investigation of fever-related potential biomarkers and metabolic pathways in the rat fever model is described in this paper. Materials and methods Rat fever model was established by dry yeast. A large number of endogenous metabolites in serum and urine were detected by UPLC-Q-TOF/MS, and fever-related potential biomarkers were screened and identified by multivariate analysis and metabolite databases. The reliability and biological significance of the largely disturbed biomarkers was verified by the metabolic network and the correlation with pharmacodynamic indicators, which contained IL-1β, IL-6, TNF-α, PGE 2 and cAMP. Results The established UPLC-Q-TOF/MS analytical method afforded satisfactory results in terms of precision, repeatability and stability, which met the requirements of biological sample determination. A total of 32 potential biomarkers associated with fever were screened and identified, among which 22 species could be adjusted by RDN. The metabolism pathway analysis revealed that valine , leucine and isoleucine biosynthesis, and sphingolipid metabolism were greatly disturbed. Their biomarkers involved L-leucine, L-valine, sphinganine and phytosphingosine , all of which showed a callback trend after RDN was given. These 4 biomarkers had a certain correlation with some known fever-related small molecules and pharmacodynamic indicators, which indicated that the selected fever-related biomarkers had certain reliability and biological significance. Conclusions RDN has a good regulation of the metabolic disorder of endogenous components in dry yeast-induced fever rats. Its antipyretic mechanism is mainly related to the regulation of amino acid, lipid and energy metabolism. The study is useful to better understand and analyze the pharmacodynamic mechanism of complex systems, such as traditional Chinese medicine.
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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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2018
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IF 2.831
Meimei Cheng,Huan Wu,Hongfei Wu,Xiaochuang Liu,An Zhou
The direct cause of hepatolenticular degeneration (HLD) is copper metabolic disorder caused by autosomal recessive inheritance. Gandou decoction (GDD), a classical traditional Chinese medicine formula, exhibits unambiguous therapeutic effect on HLD in China for decades. However, the mechanism of effect on HLD is not clear. With this purpose, the effects of copper content and histopathology inspection on the HLD rat model were investigated. Then, metabolomics study based on ultra-performance liquid chromatography quadrupole-time-of-flight mass spectrometry (UPLC-Q-TOF/MS E ) analysis and multivariate statistical analysis was adopted to further reveal the mechanism of action of GDD against HLD. The results showed that the characteristics of liver tissues after GDD treatment were significantly reversed, close to the control group, suggesting that GDD has a therapeutic effect on HLD. Furthermore, HLD interferes with 2 metabolites of the metabolic pathway in rats. Among them, up-regulation of Lactic acid, Tryptophan, Phenylalanine, Triacylglycerol and down-regulation of Linoleic acid, Alpha Linolenic acid, Phosphatidylcholine, Taurine is particularly significant. Analysis of metabolic pathways by a unique pathway analysis revealed significant changes in several pathways including lipid metabolism, amino metabolism and glucose metabolism in HLD. This study showed that GDD could provide satisfactory therapeutic effects on HLD and metabolomics study can be utilized to further understand the molecular mechanisms.
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Food Additives and Contaminants Part A-Chemistry Analysis Control Exposure & Risk Assessment
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2018
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IF 2.129
Chuan Zhou,Dianping Ma,Wenming Cao,Haiming Shi,Yuanrong Jiang
Capsaicinoids are pungent components in hot peppers, which have been detected in waste cooking oil. However, trace analysis of capsaicinoids in edible and crude vegetable oils is a challenging task due to the complex matrix. In this study, a simple liquid-liquid extraction and solid phase extraction (SPE) coupled with RP-UPLC-ESI-MS/MS method was developed for the quantification of capsaicinoids in edible and crude vegetable oils to screen the adulteration with waste cooking oil. This method was used to simultaneously determine 3 capsaicinoids (capsaicin, dihydrocapsaicin, and nordihydrocapsaicin) with capsaicin-d3, and dihydrocapsaicin-d3 as internal standards. This method allows the complete analysis of a sample in only an hour, even including sample preparation and chromatographic separation. The linear range of 3 capsaicinoids ranged between 0.5 and 40 µg/kg. The limit of detection (LOD) and limit of quantification (LOQ) for capsaicinoids were calculated as 0.15 and 0.5 µg/kg, respectively. Quantitative recoveries ranging from 92.9% to 105% were obtained by the analysis of spiked oil. The relative standard deviations were less than 5% (n = 6). The established method can potentially overcome the interference of triacylglycerols and fatty acids in edible and crude vegetable oils, and have been successfully applied to analyse real oil samples. This method provided a rapid and reliable method for the detection of adulteration of vegetable oils with waste cooking oils.
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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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2015
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IF 2.979
Yang Li,Guisheng Zhou,Ying Peng,Pengfei Tu,Xiaobo Li
Acteoside, isoacteoside, and 2′-acetylacteoside are three representative phenylethanoid glycosides (PhGs), which are widely distributed in many plants and also known as the active components of Cistanches Herba . However, the extremely low oral bioavailability of acteoside in rats implies that these structural similar components may go through multiple sequential routes of hydrolysis in gastrointestinal tract before they are absorbed into blood. Therefore, the metabolites of these three components and other PhGs from gastrointestinal tract such as echinacoside, are supposed to be the bioactive elements. In this study, we established an approach combining ultra-performance liquid chromatography/quadrupole time-of-flight mass spectrometry (UPLC/Q-TOF-MS) with MS E technology and MetaboLynx™ software for the rapid metabolic profiling of acteoside, isoacteoside, and 2′-acetylacteoside by human intestinal bacteria. As a result, 11 metabolites of acteoside, 7 metabolites of isoacteoside, and 11 metabolites of 2′-acetylacteoside were identified respectively. 8 metabolic pathways including deglycosylation, de-rhamnose, de-hydroxytyrosol, de-caffeoyl, deacetylation, reduction, acetylation, and sulfate conjugation were proposed to involve in the generation of these metabolites. Furthermore, we found that the degraded metabolites hydroxytyrosol (HT) and 3-hydroxyphenylpropionic (3-HPP) were transformed from acteoside, isoacteoside, and 2′-acetylacteoside by human intestinal bacteria and demonstrated similar bioactivities to their precursors. These findings are significant for our understanding of the metabolism of PhGs and the proposed metabolic pathways of bioactive components might be crucial for further pharmacokinetic evaluations of Cistanches Herba .
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BIOMEDICAL CHROMATOGRAPHY
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2014
·Vol. 28
·期 10
·1325-1334
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IF 1.662
Zhangxiao Peng,Yan Wang,Xue Gu,Xiaojie Guo,Chao Yan
A method based on high-performance liquid chromatography coupled with ultraviolet detection was developed for studying the pharmacokinetics of costunolide (Cos) and dehydrocostus lactone (Dehy) in rats after intravenous (i.v.) administration. Following i.v. administration, the maximum plasma concentrations of Cos and Dehy were observed to be 12.29 ± 1.47 and 5.79 ± 0.13 µg/mL, respectively. The bioavailability of Cos was larger than that of Dehy; however, the clearance and the volume of distribution of Dehy were much larger than those of Cos. An ultraperformance liquid chromatography/quadrupole time-of-flight mass spectrometry system with automated MS E (E represents collision energy) data analysis software (MetaboLynx TM ) was used to analyze and identify the metabolites of Cos and Dehy in vivo . Four metabolites of Cos and six metabolites of Dehy were discovered from the plasma, urine and feces of rats. The main metabolic pathway of Cos was phase II biotransformation, but the main metabolic pathways of Dehy was phase І biotransformation. Two sequential desaturations and N -acetylcysteine conjugation were the common metabolic pathways of Cos and Dehy in rats. This information may be useful for the further development of the two drug candidates. Copyright © 2014 John Wiley & Sons, Ltd.
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
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2024
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IF 2.8
Peng Wang,Qiuliang Xu,Hua Zou,Ming Liu,Xiangjing Gao,Hong Ren,Junlin Wang,Yiyao Cao
Accurate, reliable, and sensitive methods for the determination of eight metabolites of p-chloronitrobenzene (p-CNB) were developed based on ultra-performance liquid chromatography − quadrupole − orbitrap high resolution mass spectrometry (UPLC-Q-Orbitrap HRMS). The free and conjugated forms of metabolites were determined before and after urine samples were hydrolyzed with acid. Subsequently, three solid phase extraction steps were used for concentration and purification. The calibration curves of the eight metabolites exhibited good linearity with an R 2 of >0.999, and the precision was good as well, with the coefficient of variations of intra-day and inter-day being lower than 7.0 % and 8.5 %, respectively. Analytical accuracy for all metabolites varied within ranges of 76.0–102.9 %, and the limit of detection and limit of quantification of all the metabolites varied within ranges of 0.2–7.7 μg/L and 0.6–25.6 μg/L in human urine, respectively. In addition, the application potential of the proposed methods were evaluated by applying them to the determination of metabolites in the urine of workers exposed to p-CNB, and these results showed that these methods were accurate, reliable, and sensitive, which makes them an excellent choice for detecting the metabolites of p-CNB in the urine of exposed workers.
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Frontiers in Chemistry
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2025
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IF 4.2
Lingguo Zhao,Ronggui Lv,Jiang Song,Xi Chen,Lei Lei,Weixian Zeng,Miaowen She,Dabing Li,Xiaxia Yu,Zhanguo Liu,Xiao Wang,Yong Liu
A UPLC-MS/MS method with one-step extraction and simultaneous determination of bongkrekic acid (BA) and dehydroacetic acid (DHA) in rice noodles has been established in this study for the first time. The extraction solvent consisted of a mixture of methanol, ammonia, and water. Electrospray ionization negative ion mode (ESI-) was used for multiple reaction detection and external standard method was used for quantitative determination. The method demonstrated a good linearity range of 0–50 ng/mL with a correlation coefficient (r) of 0.9998 for BA, and showed a linearity range of 0∼500 ng/mL with r of 0.9993 for DHA. The limits of detection (LOD) were determined to be 0.1 μg/kg for BA and 0.6 μg/kg for DHA. Additionally, the method exhibited good recovery of 90.1%∼105.4% for BA and 80.4%∼102% for DHA. Meanwhile, the method also exhibited good precision with RSD of 0.4%∼7.5% for BA, and with RSD of 4.5%∼11.4% for DHA. Furthermore, the established method was sucessfully applied to the analysis of rice noodles from two production enterprises. BA was detected in one rice noodle sample and DHA was detected in 7 rice noodle samples in the enterprises A which was the manufacturer of food consumed by the poisoned patient. To investigate the cause of death of the poisoned patient, the toxigenic bacterium Burkholderia gladiolus was isolated and cultured to produce BA. The results showed that the established method could also be used to qualitatively screen BA and its isomer isobongkrekic acid (IBA) in GVC enrichment broth, potato glucose agar and rice sample, which facilitates a rapid and accurate judgement of whether the isolated bacterium strain produces BA. With high sensitivity and accuracy, and simple sample pretreatment, the proposed method shows potential for safety assessment of the entire production process of rice-derived products, addressing a significant public health concern.
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FOOD CHEMISTRY
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2024
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IF 8.5
Tianxing Wang,Wei Liu,Ling Chen,Xiaoxi Li
Foodborne heterocyclic aromatic amines (HAAs) are potent mutagens and carcinogens, posing significant health risks. Existing enrichment methods for HAAs need better adsorption selectivity and capacity for daily exposure assessment. This study hypothesized that introducing carboxylic groups into magnetic covalent organic frameworks (m-COFs) would improve HAAs adsorption by providing additional binding sites. Hence, we prepared a novel magnetic adsorbent, termed as Fe 3 O 4 @DOPA-TpPa-(COOH) 2 capable of enhancing the HAAs detection through magnetic solid-phase extraction (MSPE) coupled with UPLC-MS. This sorbent demonstrated a large specific surface area (130.7 m 2 /g), high magnetic responsivity (21.05 emu/g), and robust stability, with an adsorption capacity (Qm[cal]: 81.82 mg/g) driven by electrostatic, LP − π/C-H − π interactions, and hydrogen bonding. Optimal MSPE conditions provided sensitive detection with a broad linear range (5–500 ng/mL), low limits of detection (0.01–7.01 ng/g), and excellent repeatability. Application to Cantonese mooncake samples showed satisfactory recoveries (62.12%–126.86%). This method offers a more accurate tool for detecting HAAs.
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Arabian Journal of Chemistry
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2024
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IF 5.3
Dong Xie,Guangfu Lv,Yuchen Wang,Wenjing Zhang,Nian Li,Yao Duan,Qing Huang,Ge Chen,Zifeng Pi,Hao Yue
Tenghuang Jiangu Wan (THJGW) is a commonly utilized treatment for osteoarthritis (OA), yet its pharmacodynamic material basis and molecular mechanism remain inadequately understood. This study systematically characterized the in vitro and in vivo chemical components of THJGW using ultra-performance liquid chromatography-quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF-MS). The pharmacodynamic material basis of THJGW in the treatment of OA was explored through a target network pharmacology approach and molecular docking technology. Cellular experiments were subsequently employed to validate the molecular mechanisms. Consequently, a total of 134 components from THJGW were identified in vitro , comprising 45 flavonoids, 10 iridoid glycosides, 39 phenylethanoid glycosides, 9 phenylpropanoids, 11 organic acids, 4 phenolics, and 16 other compounds. Additionally, 38 prototype absorbed components in serum were characterized for the purpose of network construction. 11 key components and 10 core targets (VEGFA, STAT3, RELA/NF-κB p65, PIK3R1, PIK3CA, MMP9, MMP1, IL-6, HDAC1, and FGF2) were determined by the target network pharmacology. Through Gene Ontology (GO) enrichment and Kyoto Encyclopedia of Genes and Genomes (KEGG) pathway analysis, it was found that these intersection targets are associated with various signaling pathways such as pathways in cancer, lipid and atherosclerosis, and prostate cancer. Notably, the lipid and atherosclerosis pathway was closely linked to OA. The molecular docking results demonstrated strong binding affinities of the three core targets: IL-6, STAT3, and RELA/NF-κB p65. These results suggest that these targets may play a significant role for THJGW in treating OA. In vitro experiments showed that THJGW had notable protective effects on LPS-induced RAW264.7 macrophages by reducing levels of TNF-α and IL-6, and inhibiting phosphorylation expression of STAT3 and NF-κB p65 proteins related to the lipid and atherosclerosis pathway. This study provides insight into the pharmacodynamic material basis and mechanism of action for THJGW in the treatment of OA, which provide scientific evidence for the scientific application and improvement of quality standards for THJGW.
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CHEMISTRY & BIODIVERSITY
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2024
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IF 2.3
Xinhui Fan,Ke Li,Xuemei Qin,Zhenyu Li,Yuguang Du
Astragali Radix polysaccharides (APSs) exhibit a broad spectrum of biological activity, which is mainly related to immune regulation. At present, most available studies focus on total APSs or a certain component of APSs. However, structural structure study and screening for the anti-inflammatory activity of polysaccharides with different molecular weights (MW) have yet to be conducted. In this study, lipopolysaccharide (LPS)-induced RAW264.7 macrophages were used as a model to investigate the anti-inflammatory activity of APSs and its fractions. The results revealed that fraction APS-I had better anti-inflammatory effects than APS-II. After APS-Ⅰ was hydrolyzed by trifluoroacetic acid (TFA), the resulting degradation products oligosaccharides were fully methylated. These derivatized oligosaccharides were further analyzed by MALDI-TOF-MS and UPLC-Q-Exactive-MS/MS. The results showed that APS-Ⅰ was a hetero-polysaccharide with a molecular weight of about 2.0 × 106 Da, mainly consisting of glucose (46.8%) and galactose (34.4%). The degree of polymerization of Astragali Radix oligosaccharides (APOS) was 2-16. APOS were identified as 1,4-glucooligosaccharides and 1,4-galactooligosaccharides. The findings of this study lay the foundation for further elucidation of structure-function relationships of APSs and provide guidance for the development of anti-inflammatory drugs.
研究领域:
药理学
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生物化学
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免疫学
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FOOD CHEMISTRY
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2026
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IF 10.4
Sumei Ru,Jiaxin Li,Yingshuang Lu,Yan Zhang,Junping Wang,Lu Dong,Shuo Wang
Developed UPLC-MS/MS for 8 free/cross-linked AGEs quantitation. • Achieved LODs 0.8–2.5 μg/L, surpassing prior reports. • Assessed AGEs in meat products, showing processing impacts. A universal ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed for the simultaneous detection of eight free- or cross-linked advanced glycation end products (AGEs), including Nε-carboxymethyllysine, Nε-carboxyethyllysine, N δ -(5-hydro-5-methyl-4-imidazolon-2-yl)ornithine, glyoxal-derived hydroimidazolone, methylglyoxal lysine dimer, glyoxal lysine dimer, pyrraline and argpyrimidine. This method achieved the separation and quantification of the eight AGEs substances within 16 min. All analytes exhibited high correlation coefficients (R 2 > 0.999) within their respective linear ranges. Limits of detection and quantification in reconstituted solution were 0.8–2.5 and 2.5–5.5 μg/L, corresponding to 0.08–0.25 and 0.25–0.55 mg/kg in samples. Respectively. Method validation was performed using crispy fried pork as a blank matrix. The recovery rates ranged from 85.5% to 122.0%, with acceptable intra-day and inter-day precision. This method was successfully applied to the detection of AGEs in 30 different representative meat products, providing technical support for the research on the formation and control of AGEs.
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