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ANALYTICA CHIMICA ACTA · 2022 · IF 6.911

MIL-88B(Fe)/cellulose microspheres as sorbent for the fully automated dispersive pipette extraction towards trace sulfonamides in milk samples prior to UPLC-MS/MS analysis

Lin Li,Hongyu Zhang,Mengdan Zhang,Ting Wang,Xiaohong Hou

MIL-88B(Fe)/cellulose microspheres (MIL-88B(Fe)/CMs) were characterized by the means of SEM, XRD, TGA and N 2 adsorption-desorption test. The composite was used as the sorbent for fully automated dispersive pipette extraction (DPX), after introducing CMs as the support, the loss of MIL-88B(Fe) in DPX was avoided. Coupled to UPLC-MS/MS, the proposed method was employed for the analysis of trace sulfonamides (SAs) in milk samples. The parameters affecting the extraction efficiency, including pH of sample solution, the rate of aspiration and dispense, amount of the adsorbent, type and volume of elution solvent were optimized. Under the optimal conditions, good linearity (r ≥ 0.9978 for five analytes), high sensitivity (limit of detection: 0.00660–0.0136 μg kg −1 ) and satisfactory recovery (69.8%–100.9%) were achieved. Furthermore, the sorbent showed desirable reusability over eight extraction cycles. Compared with other methods for the pretreatment of SAs, the proposed method showed advantages of high sensitivity, less sorbent consumption, environmental friendliness and automation, providing a promising protocol for sample preparation.

研究领域: 分析化学 · 食品科学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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Frontiers in Pharmacology · 2024 · IF 4.4

Exploration of chemical compositions in different germplasm wolfberry using UPLC-MS/MS and evaluation of the in vitro anti-inflammatory activity of quercetin

Lan Tian,Duan Guozhen,Qi Youchao,Almezgagi Maged,Fan Guanghui,Ma Yonggui

Wolfberry, esteemed as a traditional Chinese medicinal material and functional food, is replete with nutrients and boasts a diverse array of health benefits, including hypoglycemic, antitumor, antioxidant, anti-inflammatory, and immune-enhancing properties. Notably, inflammation is a pivotal factor in the onset and progression of numerous diseases. Despite this, there is a paucity of research on the comprehensive evaluation of the components found in different wolfberries, and the exploration of their primary active components is limited. To address this issue, we conducted a comprehensive targeted metabolomics analysis, employing statistical methods such as principal component analysis (PCA), orthogonal partial least squares discriminant analysis (OPLS-DA), KEGG pathway analysis, and volcano plots to delineate the compositional differences among red, black, and yellow wolfberries. Furthermore, we investigated the anti-inflammatory effects of their primary components through in vitro experiments. Our analysis revealed a total of 1,104 chemical compositions in the three wolfberries, with alkaloids, phenolic acids, flavonoids, and lipids being the predominant nutritional components. KEGG enrichment analysis indicated that these compositions were primarily involved in the biosynthesis of secondary metabolites, ABC transport, and galactose metabolism pathway. Moreover, our study demonstrated that quercetin exhibited dose-dependent anti-inflammatory activity in LPS-stimulated HUVECs. It effectively inhibited the production of inflammatory factors such as TNF-α, MCP-1, and IL-1β, while also down-regulating the gene and protein expression levels of ICAM-1 and VCAM-1. In conclusion, our findings indicate that there are variations in compositions among the three wolfberries, with flavonoids being the most abundant, and in vitro studies also confirmed the anti-inflammatory potential of quercetin. It is worth noting that Lycium ruthenicum contains higher levels of antioxidant components and possesses greater nutritional value, providing valuable insights for the future development and utilization of the three wolfberries.

CAS / MDL: 64-18-6
研究领域: 药理学 · 代谢组学 · 生物化学 · 药物化学 · 植物科学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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MICROCHIMICA ACTA · 2017 ·Vol. 184 ·期 8 ·2981-2990 · IF 4.58

Magnetic solid phase extraction of non-steroidal anti-inflammatory drugs from water samples using a metal organic framework of type Fe3O4/MIL-101(Cr), and their quantitation by UPLC-MS/MS

Wang Ting,Liu Siyu,Gao Guihua,Zhao Pan,Lu Nan,Lun Xiaowen,Hou Xiaohong

The authors describe a method for magnetic solid phase extraction (MSPE) combined with ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) for the quantitation of eight non-steroidal anti-inflammatory drugs (NSAIDs) in wastewater and environmental water samples. Specifically, the NSAIDs were directly extracted by using a magnetic nanocomposite of type Fe 3 O 4 /MIL-101(Cr) (Matérial Institute Lavoisier, MIL) from 50 mL water samples without any further cleanup. The effects of the amount of adsorbent, pH value, salt concentration, ultrasonic extraction time, desorption solvent nature and volume and desorption time were investigated. Under the optimal conditions, UPLC-MS/MS based detection resulted in the following figures of merit: (a) Linear calibration plots that typically extend from 0.1 (0.2, 0.05, 0.02) to 50 μg·L −1 , depending on the compound; (b) detection limits between 3 to 60 ng·L −1 ; and (c), recoveries varying from 81.2% to 116.8% with relative standard deviations between 0.4% and 10.8%. The adsorption of NSAIDs on Fe 3 O 4 /MIL-101(Cr) was characterized by adsorption isotherms, kinetics and thermodynamics studies and provides a deeper insight into the adsorption mechanism. Compared to other method for pretreatment and preconcentration of NSAIDs, the new method is more rapid, sensitive, accurate and eco-friendly. The method was successfully applied to the determination of the NSAID residues in a variety of real environmental and wastewater samples. Schematic of a method for determination of non-steroidal anti-inflammatory drugs (NSAIDs) in environmental water by magnetic solid phase extraction based on Fe 3 O 4 /MIL-101(Cr) combined with UPLC-MS/MS. The adsorption mechanism of NSAIDs on Fe 3 O 4 /MIL-101(Cr) was studied.

CAS / MDL: 1317-61-9
研究领域: 环境科学 · 分析化学
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ENVIRONMENTAL SCIENCE AND POLLUTION RESEARCH · 2022 ·Vol. 30 ·期 10 ·27357-27371 · IF 5.19

Simultaneous trace determination of three natural estrogens and their sulfate and glucuronide conjugates in municipal waste and river water samples with UPLC-MS/MS

Ma Qing-guang,Wan Yi-ping,Liu Ze-hua,Dang Zhi

Analytical method for three natural estrogens (NEs) and their sulfate and glucuronide conjugates in waste and river waters using solid-phase extraction (SPE) coupled with ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) has been available, but problems including poor recovery exist. In order to solve these, some optimizations have been performed in this work. For sample preparation, both rinse and elution solutions were optimized, in which 6 mL of MeOH/water (1:9, v/v), MeOH/Ace/water (10:2:88, v/v/v), and MeOH/NH 4 OH/water (10:2:88, v/v/v) were determined as the rinse solution, while 6 mL of 2.0% NH 4 OH/MeOH was determined as the elution solution for conjugated NEs (C-NEs). For mobile phase, addition of NH 4 F could obviously enhance the signal response of the nine target compounds, and the optimized addition concentration was 0.5 mmol/L. The developed efficient method was validated and showed excellent linearity for each target compound ( R 2  > 0.998), low limit of quantifications (LOQs, 0.07–1.29 ng/L) in four different water matrices, and excellent recovery efficiencies of 81.0–116.1% in influent, effluent, ultra-pure, and river water samples with low relative standard deviations (RSDs, 0.6–13.6%). The optimized method was successfully applied to influent, effluent, and Pearl River water, among which three NEs were all detected, while five C-NEs were found in the influent, three C-NEs were detected in the effluent, and two C-NEs were found in the Pearl River water, indicating the wide distribution of NEs and C-NEs in different water environments. This work provided a reliable and efficient analytical method for simultaneous trace determination of NEs and C-NEs, which had satisfactory absolute recoveries with low RSDs, low LOQs, and time-saving for both analysis and nitrogen drying.

CAS / MDL: 64-19-7
研究领域: 环境科学 · 分析化学 · 水质
✓ 已验证 产品关联 DOI PubMed 高影响因子
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FOOD CHEMISTRY · 2021 · IF 7.514

Rapid determination of multi-antibiotic residues in honey based on modified QuEChERS method coupled with UPLC–MS/MS

Yan Yang,Guobing Lin,Lijing Liu,Tainan Lin

Antibiotic residues in honey cause public health problems. To analyze multi-antibiotic residues in honey, a modified QuEChERS (quick, easy, cheap, effective, rugged and safe) extraction method coupled with ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) was developed for simultaneous quantification of 70 antibiotic residues in honey. Matrix-matched calibrations indicated the correlation coefficients were higher than 0.998. The recovery was in a range of 70.5%-119.8% with intra-day relative standard deviation (RSD) of ≤ 10.0% and inter-day RSD of ≤ 13.9%. The limits of detection ranged between 0.050 μg/kg and 1.02 μg/kg. Limits of quantification was 0.17 μg/kg to 3.40 μg/kg. The matrix effects were negligible in 71.4% of compounds and moderately in 24.3% of compounds. Methacycline, oxytetracycline, tetracycline and its metabolite 4-tetracycline residues were detected in the tested samples. Validation parameters were acceptable and were in line with the Codex guidelines. This method was effective for detecting multi-antibiotic residues in honey.

CAS / MDL: 139-33-3
研究领域: 食品科学 · 分析化学 · 公共卫生
✓ 已验证 产品关联 DOI PubMed 高影响因子
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FOOD CHEMISTRY · 2019 · IF 5.399

Evaluation of cellular antioxidant components of honeys using UPLC-MS/MS and HPLC-FLD based on the quantitative composition-activity relationship

Shi Shen,Jingbo Wang,Xi Chen,Tingting Liu,Qin Zhuo,Shuang-Qing Zhang

Antioxidant molecules in honey contributed to various biological effects, but antioxidant components markers in honey are required to be investigated further. Phenolic compounds, flavonoids and free amino acids were analyzed using UPLC-MS/MS and HPLC-FLD from 39 honey samples, in which fennel honey was firstly investigated. Based on the quantitative composition-activity relationship, the cellular antioxidant activity (CAA) assay of various honeys is closely related with the interaction of some phenolic compounds (isoferulic acid, 3,4-dihydroxy benzoic acid, 4-hydroxy benzoic acid, chlorogenic acid, caffeic acid, gallic acid, cryptochlorogenic acid, p -coumaric acid, salicylic acid), flavonoids (isosakuranetin, sakuranetin, pinocembrin, vitexin, taxifolin, galangin, luteolin, chrysin) and free amino acids (Tyr, Gly, Ile, Glu, Val, Phe, Leu, Asp, His, Pro, Ala). The results would be beneficial for the understanding of the nutritional values, exploitation and utilization of honeys with different floral origins, further contributable to the market development and consumption choice of honey.

研究领域: 食品科学 · 分析化学 · 药理学 · 营养学
✓ 已验证 DOI PubMed 高影响因子
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RSC Advances · 2016 ·Vol. 6 ·期 114 ·113209-113218 · IF 3.289

Simultaneous determination of paeoniflorin-6′-O-benzene sulfonate (CP-25) and its active paeoniflorin (Pae) metabolite in rat plasma using UPLC-MS/MS: an application for pharmacokinetic studies

Jun Yu,Feng Xiao,James Asenso,Peng Zhou,Xiao-Dan Yang,Chun Wang,Wei Wei

Paeoniflorin (Pae), a water-soluble monoterpene glucoside, is the main effective component of total glucoside of paeony (TGP). Pae has a very low bioavailability (3.6%). The aim of this study was to investigate the effects of sex, food and disease status on the pharmacokinetics of paeoniflorin-6′-O-benzene sulfonate (acylated derivative of Pae, CP-25) and its primary metabolite (Pae, M1) after oral administration in the plasma of rats. A specific and sensitive ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) assay for rapid determination of CP-25 and Pae in rat plasma was developed and validated for the first time. The assay was validated in terms of selectivity, linearity, accuracy, precision, recovery, matrix effects and stability. We found that CP-25 had a more extensive distribution in females than that in males, but no differences in M1 levels were found. Food intake could also increase the extent of absorption and decrease the rate of clearance for CP-25 and M1 after oral administration in rats. The disease status would decrease the absorption of CP-25 in rats. Comparing single-doing and multiple-dosing in an adjuvant arthritis (AA) model, the absorption of CP-25 and M1 improved with increasing dosage. Furthermore, during the period of multiple-dosing, CP-25 exhibited a better anti-inflammatory effect in AA rats and no obvious side effects occurred during the dosing period. Our findings provide the basis, and some guidelines, for further studies into the clinical application of CP-25.

CAS / MDL: 9004-32-4 120-47-8
研究领域: 药理学 · 分析化学 · 临床医学
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INTERNATIONAL JOURNAL OF BIOLOGICAL MACROMOLECULES · 2025 · IF 8.5

Simultaneous determination of the monosaccharide types and their absolute configurations in polysaccharides based on UPLC-MS/MS

Yongchun Huang,Jie Bai,Jinman Shui,Zhanhai Su,Chengzhu Cao,Haiyan Wang,Qiong Wu,Shoude Zhang

Analysing monosaccharide composition is an essential step in deciphering polysaccharide structures. However, it presents significant challenges due to the pronounced hydrophilicity and the vast array of monosaccharide isomers. Gas/liquid chromatography, coupled with an aldononitrile acetate derivatisation, has been widely used for monosaccharide composition analysis. However, it poses considerable difficulties in simultaneously determining the D/L configurations of these monosaccharides. In this study, a novel method that can simultaneously determine the composition of polysaccharides and their D/L configuration based on L-cysteine methyl ester derivatisation (CMED) and ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) is developed for the comprehensive analysis of monosaccharide types. This method enables the simultaneous characterization of aldoses, ketoses, alditols, and uronic acids. Furthermore, the reaction mechanisms and by-products were meticulously analysed, offering a robust theoretical basis for this novel methodology. Additionally, the developed method was employed to characterize the monosaccharide composition for six plant polysaccharides. Ultimately, the findings demonstrated that the proposed method is effective for confirming monosaccharide composition, encompassing both structural types and absolute configurations.

研究领域: 分析化学 · 碳水化合物化学 · 生物化学 · 植物科学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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ANALYTICAL AND BIOANALYTICAL CHEMISTRY · 2018 ·Vol. 410 ·期 25 ·6619-6632 · IF 3.307

Development and application of metal organic framework/chitosan foams based on ultrasound-assisted solid-phase extraction coupling to UPLC-MS/MS for the determination of five parabens in water

Li Shuo,Jia Mengtian,Guo Hongqiao,Hou Xiaohong

In this work, a variety of highly porous metal organic framework/chitosan (MOF/CS) foams (MIL-53(Al)/CS, MIL-53(Fe)/CS, MIL-101(Cr)/CS, MIL-101(Fe)/CS, UiO-66(Zr)/CS, and MIL-100(Fe)/CS) were designed and prepared by an ice-templating process. The introduction of MOFs made these foams achieve excellent inherent characters in terms of strength, stability, and adsorption ability. The MOFs incorporated in the foams retained their unique properties. Additionally, the foams were durable and their adsorption abilities had only a little loss after being recycled several times. MIL-53(Al)/CS foam was selected as an adsorbent candidate to develop an ultrasound-assisted solid-phase extraction (UA-SPE) method for the first time, owing to its particularly noteworthy performance among the prepared MOF/CS foams. The method was then successfully applied to extract trace amount of five parabens (methylparaben, ethylparaben, propylparaben, butylparaben, benzylparaben) in water samples, followed by ultra-performance liquid chromatography coupled with tandem mass spectrometry (UPLC-MS/MS) detection. Several experimental parameters were investigated. Under the optimal conditions, the linear ranges were 0.5–200 μg/L with regression coefficients ( r 2 ) from 0.9948 to 0.9983. The method detection limits were between 0.09 and 0.45 μg/L. The recoveries ranged from 78.75 to 102.1% with relative standard deviations (RSDs) < 7.4%. Furthermore, the molecular interactions and free binding energies between MOFs and parabens were calculated by means of molecular docking to explain the adsorption mechanism deeply. The novel method proposed in this work exhibited many benefits such as easy operation, high enrichment efficiency, less solvent consuming, and higher sensitivity. Such a strategy would expand the application prospect of MOFs in sample pretreatment. ᅟ

研究领域: 环境科学 · 分析化学
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JOURNAL OF CHROMATOGRAPHY A · 2025 · IF 4

Determination of perfluoroalkyl carboxylic acids in mice serum and tissue by dispersive solid-phase extraction based on fluorine-functionalized covalent organic frameworks coupled with UPLC-MS/MS

Jinni Zhang,Songtao Li,Xiaojing Li,Canrong Chen,Wen Xie,Yanhui Zhong,Zian Lin,Zongwei Cai

Perfluoroalkyl carboxylic acids (PFCAs) are a class of persistent organic pollutants (POPs), which posed various hazards to organisms, including reproductive, developmental, neurological, and immunological toxicity. Consequently, developing an analytical method aimed at achieving highly sensitive detection of trace amounts of PFCAs in complex samples is clearly of great significance. Herein, the Fluorine-functionalized covalent organic framework (F-COF) was synthesized at ambient temperature, which has the advantages of high specific surface area (1297.7 m 2 g -1 ), suitable selective adsorption pore size and good stability. Based on the multiple effects of suitable pore size, fluorine-fluorine interactions and hydrophobic interactions, F-COF exhibited high adsorption performance towards PFCAs. Accordingly, the method of F-COF-based dispersive solid-phase extraction (dSPE) coupled with UPLC-MS/MS was developed for the quantitative analysis of 5 PFCAs in complex biological samples. The results showed that the good linearity for the 5 PFCAs within the concentration ranges of 0.4 to 10 4 ng L -1 , with correlation coefficients (r) all greater than 0.9993. The enrichment factors (EFs) ranged from 11.4 to 22.3 folds, and the limits of detection (LODs) were 0.11 to 0.17 ng L -1 . The established method provided a powerful tool for the enrichment and detection of PFCAs in mice serum and tissue. F-COF holds promising application prospects as a solid-phase extraction material for efficient enrichment separation and detection of PFCAs.

研究领域: 分析化学 · 环境科学 · 毒理学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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JOURNAL OF ETHNOPHARMACOLOGY · 2025 · IF 5.4

Potential components and action mechanism of Tongzhi Surunjiang Pills against acute gouty arthritis: UPLC-MS/MS, network pharmacology, molecular docking, and transcriptomic analysis

Wanting Fu,Aoqi Ye,Huimin Yang,Xia Hou,Zhongjing Wang,Zhun Hu,Xiang Yu,Xindi Li,Zejun Yu,Yang Li,Yinsheng Qiu,Zhinan Mei,Lingyun Xu

Ethnopharmacological relevance Gouty arthritis (GA) is a disease caused by the malfunction of purine and/or uric acid metabolism. Tongzhi Surunjing Pills (TZSRJP), a traditional Chinese medicine formula derived from the ancient Uyghur book “Karzhibadin Kadeer”, is used clinically to treat GA, which still needs more research in its complex regulatory mechanisms. Aim of study The aim of the study was to elucidate the main potential active components of TZSRJP and the mechanism by which it treated GA. Methods We used network pharmacology and molecular docking to predict possible active ingredients and targets, and UPLC-MS to identify the content of key components, followed by transcriptomics to analyze targets of action and also demonstrated our hypothesis in rats. Results Network pharmacology showed that TZSRJP Contained 120 active components and 934 potential targets. 9 of major active ingredients, such as gallic acid, colchicine, senoside A, and so on were identified and quantified by UPLC-MS. KEGG predicted the therapeutic effects mainly through NOD-like receptor pathway, Toll-like receptor pathway, and NF-κB pathway; molecular docking showed that its main active ingredients had high affinity with inflammation-related proteins such as NLRP3, IL-1β, and TNF. Transcriptomics also verified that the therapeutic effects were mainly carried out through inflammatory pathways. In vivo experiments verified the efficacy of TZSRJP in the treatment of GA and reduced the expression of proteins and genes related to the NLRP3 pathway. Therefore, TZSRJP alleviates GA development through the NLRP3 pathway, and the main components contain colchicine, gallic acid, and so on.

CAS / MDL: 64-18-6 67-56-1
研究领域: 药理学 · 民族药理学 · 生物信息学 · 分子生物学 · 药物化学 · 免疫学 · 分析化学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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TALANTA · 2017 · IF 4.162

A combination of computational−experimental study on metal-organic frameworks MIL-53(Al) as sorbent for simultaneous determination of estrogens and glucocorticoids in water and urine samples by dispersive micro-solid-phase extraction coupled to UPLC-MS/MS

Guihua Gao,Sijia Li,Shuo Li,Yudan Wang,Pan Zhao,Xiangyu Zhang,Xiaohong Hou

In this work, computational and experimental methods were used to study the adsorption of estrogens and glucocorticoids on metal–organic frameworks (MOFs). Computer-aided molecular simulation was applied to predict the adsorption of eight analytes on four MOFs (MIL-101(Cr), MIL-100(Fe), MIL-53(Al), and UiO-66(Zr)) by examining molecular interactions and calculating free binding energies. Subsequently, the four water-stable MOFs were synthesized and evaluated as adsorbents for the target hormones in aqueous solution. As the MOF exhibiting the highest adsorption capacity in both computations and experiments, MIL-53(Al) was chosen as a sorbent to develop a dispersive micro-solid-phase extraction procedure coupled to ultra-performance liquid chromatography tandem mass spectrometry for simultaneous determination of the target analytes in water and human urine samples. Experimental parameters affecting the extraction recoveries, including pH, ionic strength , MIL-53(Al) amount, extraction time, desorption time, and desorption solvent, were optimized. The optimized method provided a linear range of 0.005025–368.6   μg/L with good correlation coefficients (0.9982 ≤ r 2 ≤ 0.9992), and limits of detection (S/N = 3) and quantification (S/N = 10) of 0.0015–1.0   μg/L and 0.005–1.8   μg/L, respectively. The analyte recoveries were in the range of 80.6–98.4% in water samples and 88.4–93.2% in urine samples. Furthermore, MIL-53(Al) showed good stability over 10 extraction cycles (RSD < 10.0%). Good agreement between experimental measurements and computational results showed the potential of this approach for elucidating adsorption mechanisms and predicating extraction efficiencies for MOFs and targets, providing new directions for the development and utilization of MOFs.

研究领域: 环境科学 · 分析化学 · 计算化学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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