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Journal of Functional Foods · 2020 · IF 3.701

Intestinal absorption and distribution of naringin, hesperidin, and their metabolites in mice

Xiao Guo,Kaikai Li,Ailing Guo,Erhu Li

In this study, an in vivo animal experiment was performed, to investigate the intestinal absorption and distribution of naringin, hesperidin, and their metabolites by using UPLC-ESI-MS/MS and HPLC-PDA analysis. The bioavailability of naringin or hesperidin in duodenum, jejunum, ileum, cecum, and colon was calculated. A total of 7 and 13 metabolites were found and tentatively identified in intestinal tissue   after orally administered naringin and hesperidin in mice, respectively. Sulfates of naringin could be absorbed by ileum and cecum, de-glycosylation metabolites could be absorbed by duodenum, and phenolic acids could be absorbed by the cecum and colon. Sulfates of hesperidin could be absorbed by duodenum and ileum, de-glycosylation metabolites could be absorbed by cecum, and phenolic acids could be absorbed by ileum, cecum and colon. Jejunum did not absorb metabolites of naringin or hesperidin. Results could be beneficial for understanding the intestinal bioactivities of naringin and hesperidin.

CAS / MDL: 75-05-8 67-56-1
研究领域: 药理学 · 生物化学 · 营养学
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STEROIDS · 2015 · IF 2.639

A new quantitation method of protodioscin by HPLC–ESI-MS/MS in rat plasma and its application to the pharmacokinetic study

Xinxin Zhang,Zengjun Guo,Jing Li,Yoichiro Ito,Wenji Sun

A specific high performance liquid chromatography tandem mass spectrometry (HPLC–MS/MS method) was established for determining the concentration of protodioscin (PG) in rat plasma after intragastric administration of its standard form. Ginsenoside Rb 1 was selected as the internal standard (IS). The plasma sample was prepared using one-step deproteinization procedure by adding three parts of acetonitrile to precipitate proteins. The chromatographic separation was accomplished on an Inersil ODS-3 C 18 column (250   ×   4.6   mm, 5   μm) with a mobile phase composed with acetonitrile and water containing 0.1% formic acid under a gradient elution mode at a flow rate of 1   mL   min −1 . A 3:1 portion of the eluent after a microsplit was detected on a triple quadrupole tandem mass spectrometer coupled with electrospray ionization (ESI) in positive ion and multiple reaction monitoring (MRM) scanning modes. The mass transitions were selected as 888.1   →   1050.2 for PG and 948.2   →   1110.3 for IS, respectively. After careful validation, the plasma samples were always stable under different storage conditions. These analytical results rendered sensitive, selective, and reliable values by this established method which displayed high accuracy, adequate extracted recoveries, and almost negligible matrix effects. This method was applied to the pharmacokinetic studies on PG level in the rat plasma and its pharmacokinetic effect. The results of our studies suggest that the present method may be a useful tool for further clinical study of PG.

CAS / MDL: 64-18-6
研究领域: 分析化学 · 药物代谢 · 生物医学
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JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY · 2022 · IF 5.895

Comparative Mass Spectrometry Analysis and Immunomodulatory Effects of Casein Glycomacropeptide O-Glycans in Bovine and Caprine Whey Powder

Yu Lu,Jie Liu,Zhenhua Li,Wenqing Li,Jing Liu,Linjuan Huang,Zhongfu Wang

Casein glycomacropeptide carries various O-glycan modifications, which, together with variations in the amino acid composition of the glycopeptide, may result in different biological activities. In this study, O-glycans of casein glycomacropeptide from bovine and caprine whey powder were qualitatively and quantitatively analyzed by LC-UV-ESI-MS/MS, and their immune activities and regulatory mechanisms were compared. O-Glycans’ total content was 1.54 times higher in bovine than in caprine glycomacropeptide. The glycoform H1N1S2 (H: hexose; N: N-acetylgalactosamine; and S: N-acetylneuraminic acid) accounted for nearly 50% of total glycomacropeptide O-glycans in bovine milk but less than 20% in caprine milk. Bovine glycomacropeptide glycosylation promoted the immune activity of RAW264.7 cells, which may be linked to a higher content of disialylated O-glycans. Glycomacropeptide from both milk sources significantly upregulated the mRNA expression of IL-1α, TNF-α, and IL-10 in RAW264.7 cells and activated the MAPK immunomodulatory signaling pathway. This study demonstrates the possible use of casein glycomacropeptide as an immunomodulatory agent.

CAS / MDL: 89-25-8
研究领域: 食品科学 · 免疫学 · 生物化学 · 分子生物学
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INDUSTRIAL CROPS AND PRODUCTS · 2026 · IF 6.4

Valorization of Euphorbia helioscopia seeds as a lipid-rich resource with anti-EMT activity: A UPLC-ESI-MS/MS-based metabolomics approach

Lili Yu,Zhonghua Li,Huawei Xin,Na Shen,Tao Yan,Yulei Cui

Euphorbia helioscopia L. is a traditional medicinal plant, whose seeds (EHS) are often discarded as agricultural waste. This study aimed to explore the metabolic profile and anti-epithelial-mesenchymal transition (EMT) potential of EHS compared with the conventional whole herb (EHQ). Using UPLC-ESI-MS/MS-based widely targeted metabolomics, 2178 metabolites were identified, with 1423 showing differential accumulation between EHQ and EHS. EHQ was rich in flavonoids, while EHS relatively enriched in lipids compared to EHQ metabolome, enriched in fatty acids such as octanoic, stearic, and octadecenoic acids. Pathway analysis highlighted disparities in lipid and flavonoid biosynthesis. In vitro assays on A549 lung cancer cells revealed that EHS extract possessed stronger cytotoxicity (IC 50 = 0.80 mg/mL) and more potently inhibited cell migration and EMT progression, evidenced by upregulated E-cadherin and downregulated N-cadherin and α-SMA. These findings position EHS as a promising candidate contributors’ lipid-rich resource for anti-EMT drug development, advocating for the valorization of underutilized plant parts in sustainable bioproduct pipelines.

CAS / MDL: 64-17-5
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Current Analytical Chemistry · 2016 ·Vol. 12 ·期 2 ·159-166 · IF 1.238

Analysis of Homocysteine in Plasma of Rats Exposed to High-fat Diet and Chronic Unpredictable Mild Stress by LC/ESI-MS/MS

Pingting Li,Zhibin Tan,Xiaoling Gao,Shuqiang Liu,Shuling Wang

Context: Homocysteine (Hcy) is an amino acid that occurs in the body as an intermediate in the metabolism of methionine and cysteine. Hcyinplasma is a disease risk factor associated with both atherosclerosis and depression. The relation between Hcy balance and complication of atherosclerosis and depression remains unclear. Determination of Hcy in plasma is important and necessary for the research on comorbidities of atherosclerosis and depression. Objective: To establish an LC/ESI-MS/MS method for measuring plasma Hcy levels in rats and to compare plasma Hcy levels in rats exposed to high-fat diet, unpredictable mild stress or its combination. Materials and Methods: Forty rats were randomized into control group, high-fat group (HFD), chronic unpredictable mild stress group (CMS) and CMS+HFD group (n=10 in each group). 8 weeks later, the rats were sacrificed and plasma was collected for determining Hcy by LC/ESI-MS/MS. All data were analyzed by using SPSS13.0 software. Results: Compared to the plasma Hcy levels of control group, neither HFD group nor CMS group had statistical significance. However, CMS+HFD group showed a significantly higher level of plasma Hcy than the other three groups. Conclusions: Only when exposed to both high fat diets and chronic unpredictable mild stress, rats showed a remarkably elevated Hcy level in their plasma, however, when exposed alone to either high fat diet or chronic unpredictable mild stress, rats had a normal Hcy level in their plasma. Our findings indicate that Hcy is increased in comorbidity of atherosclerosis and depression.

研究领域: 生物化学 · 精神病学 · 心血管研究 · 代谢组学 · 分析化学
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EUROPEAN JOURNAL OF MASS SPECTROMETRY · 2018 · IF 1

Differentiation of isomeric haloanilines by tosylation in combination with electrospray ionization mass spectrometry

Shanshan Wang,Yuanyuan Cheng,Mengmeng Chen,Kezhi Jiang

Differentiation of the isomeric haloanilines still remains a challenging and necessary analytic task due to their identical retention time in chromatography and similar mass spectra. In this work, p-tosylation of haloanilines by reaction of haloanilines with p-toluenesulfonyl chloride resulted in the corresponding N-tosyl haloanilines. Fragmentation of protonated N-tosyl haloanilines in electrospray ionization tandem mass spectrometry (ESI-MS/MS) mainly resulted in tosyl cation, haloaniline radical cation, and halohydroxyaniline radical cation. The MS/MS of the three group isomeric derivatives showed significant difference in abundance distribution of these product ions, respectively. Theoretical calculations showed that the stability of the ion-neutral complex (INC) is a key factor influencing the relative intensity of the product ions. The three group isomeric derivatives were also separated by high performance liquid chromatograph (HPLC) at conventional conditions. p-Tosylation combined tandem MS (or HPLC) technique were carried out to realize the differentiation of isomeric haloanilines.

CAS / MDL: 75-09-2 110-86-1 98-59-9
研究领域: 分析化学 · 质谱学 · 有机化学
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JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY · 2022 · IF 5.895

Production of a Natural Dihydropteroate Synthase and Development of a Signal-Amplified Pseudo-Immunoassay for the Determination of Sulfonamides in Pork

Tong He,Peng Lei Cui,Jing Liu,Cheng Feng,Jian Ping Wang

In this study, a type of magnetic photoaffinity-labeled activity-based protein profiling probe for sulfonamide drugs was first synthesized for the purpose of capturing the natural dihydropteroate synthase of Escherichia coli by using simple incubation and magnetic separation. After characterization of its identity with LC-ESI-MS/MS, this enzyme was used as a recognition reagent to develop a direct competitive pseudo-ELISA for the determination of the residues of 40 sulfonamides in pork. Because of the use of streptavidin-horseradish peroxidase and biotinylated horseradish peroxidase as a signal-amplified system, the limits of detection for the 40 drugs were in the range of 0.001–0.016 ng/mL. Compared to the steps in a conventional assay formation, the operation steps were the same, but the sensitivities increased 32–88-fold. Furthermore, the assay performances were better than the previously reported immunoassays performances for sulfonamides. Therefore, this method could be used as a practical tool for multiscreening the trace levels of sulfonamides residues in food samples.

CAS / MDL: 21312-10-7 3563-14-2
研究领域: 分析化学 · 食品科学 · 生物化学 · 药学
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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS · 2020 · IF 3.209

Transport and metabolic profiling studies of amentoflavone in Caco-2 cells by UHPLC-ESI-MS/MS and UHPLC-ESI-Q-TOF-MS/MS

Baolin Wang,Yimeng Lu,Rong Wang,Shumeng Liu,Xiaolong Hu,Hao Wang

Amentoflavone, a kind of biflavonoid existing in several medicinal plants such as Selaginella moellendorfi and Gingko biloba , possesses anti-inflammatory, antioxidant, anti-virus, anti-tumor activities. In the present study, a new reliable and sensitive UHPLC-ESI-MS/MS method was developed to determine the permeability of amentoflavone under different conditions, and its metabolites in Caco-2 cells were identified by means of UHPLC-Q-TOF-MS/MS method. The results showed that amentoflavone could be considered as a compound with moderate intestinal absorption in Caco-2 cell model and its absorption characteristics might be involved in paracellular passive penetration and clathrin-mediated endocytosis with no participation of efflux transporters. Eight metabolites of amentoflavone were identified in Caco-2 cell model, indicating that the main metabolic pathways were oxidation, reduction, methylation and glucuronide conjugation. This study can provide valuable evidence for an in-depth understanding of absorption mechanism and transformation of amentoflavone in the intestine.

CAS / MDL: 60-00-4 64-18-6 152-11-4
研究领域: 药理学 · 分析化学 · 生物化学
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MICROCHEMICAL JOURNAL · 2026 · IF 5.2

A three-tier screening strategy-based targeted UPLC-ESI-MS/MS platform delineates the FAHFA landscape in lipid extracts of fruit seeds and pits

Long Xu,Xiang Liang,Mengqing Xiao,Walter Vetter,Shuaishuai Yang,Kai Chen,Fashan Wei,Xiaoling Yu,Xia Shen,Mingjiang Zhu

A 3-tier screening strategy-based LC-MS/MS profiles FAHFAs in fruit seeds and pits. • Fruit seed oils contain significantly higher total FAHFA levels than pit oils. • Bayberry seed oil is the richest FAHFA source (168 ng/g) among all samples. • OAHOA and PAHOA are identified as predominant FAHFA species in fruit seeds. Fatty acid esters of hydroxy fatty acids (FAHFAs) are bioactive lipids with anti-inflammatory and antidiabetic properties, but their occurrence in fruit seeds and pits remain largely unexplored. Here, untargeted lipidomics and fatty acid profiling were firstly employed to characterize the overall lipid landscape and precursor pools. Subsequently, a targeted platform was established by integrating solid-phase extraction (SPE) enrichment, N , N -dimethylethylenediamine (DMED) derivatization, and UPLC-ESI-MS/MS in multiple reaction monitoring (MRM) mode. Using a predictive MRM database covering 2116 theoretical FAHFA species and a three-tier screening strategy (two MRM filtering rounds followed by retention time and signal-to-noise evaluation), 49 endogenous species were identified in 17 fruit seeds and 4 fruit pits. It was found that fruit seed oils contained significantly higher total FAHFA levels than pit oils (3–168 vs. 1–35 ng/g), with bayberry seed oil showing the highest content (168 ng/g). Predominant species included OAHOA, LAHLA, PAHOA, and OAHSA. This first comprehensive FAHFA profile, achieved via the three-tier strategy, establishes seed oils as notable dietary sources of these lipids and offers a robust platform for discovering bioactive lipids in complex plant matrices. Download: Download high-res image (113KB) Download: Download full-size image

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Analytical Methods · 2018 ·Vol. 10 ·期 10 ·1247-1257 · IF 2.073

Deep eutectic solvent-based extraction coupled with green two-dimensional HPLC-DAD-ESI-MS/MS for the determination of anthocyanins from Lycium ruthenicum Murr. fruit

Jun Sang,Bing Li,Ya-ya Huang,Qun Ma,Kang Liu,Cui-qin Li

This study aimed to extract and separate total anthocyanins from Lycium ruthenicum Murr. by combining deep eutectic solvents (DES) with macroporous resin chromatography and to develop green analytical methods for the determination of anthocyanins. Choline chloride/1,2-propanediol (1 : 2, mol mol−1) containing 10% water (v/v) was screened as the optimal extraction solvent, and extraction at 52 °C for 45 min using a liquid/solid ratio of 20 : 1 gave the maximum extraction yield of total anthocyanins (4.45 ± 0.07 mg g−1). According to the static/dynamic adsorption and desorption tests, LS-32 macroporous resin has the ability to separate anthocyanins from DES with a recovery ratio above 95%. An off-line heart-cutting two-dimensional HPLC-DAD/ESI-MS method was developed for the qualitative and quantitative analysis of L. ruthenicum anthocyanins using environmentally friendly mobile phases. Ethanol and a tartaric acid solution (0.3 mol L−1) were used as the mobile phases of the first-dimensional HPLC-DAD method, and 15 anthocyanin peaks were detected within 17 min. The second-dimensional HPLC-MS method was used to identify the main anthocyanin peaks in the first dimension. Method validation showed that the developed method was accurate, stable and reliable for the analysis of L. ruthenicum anthocyanins. The present study provides an excellent alternative green method for the preparation and determination of anthocyanins from plant material.

研究领域: 分析化学 · 植物化学 · 食品科学
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ANALYTICAL CHEMISTRY · 2024 · IF 6.7

Accurate Quantification of Ten Methylated Purine Nucleosides by Highly Sensitive and Stable Isotope-Diluted UHPLC–MS/MS

Lyuye Zhang,Weibing Zhang,Hailin Wang

The dynamic landscape of cellular nucleotides/nucleosides associated with RNA metabolism, particularly in diseases like cancer, has spurred intensive interest. Here, we report a robust stable isotope-diluted UHPLC–ESI-MS/MS method for accurate quantification of 12 purine ribonucleosides, including 10 methylated purine nucleosides. By the use of thermally decomposable ammonium bicarbonate (NH4HCO3) as a mobile phase additive for UHPLC–MS/MS detection, the ESI-MS/MS signal responses of these target compounds were enhanced by 1.7–24.5 folds. Noteworthily, three methylated guanosine isomers (m1G, m2G, and m7G) and two methylated adenosine isomers (m1A and m6A) that are indistinguishable directly by mass spectrometry were well resolved with optimal UHPLC separation. Combined with methanol extraction and solid-phase extraction (SPE) pretreatment, the method quantified intracellular concentrations of three modified nucleosides (Gm, m1G, and m2G), which would otherwise be undetectable because of significant suppression of their signals by the interfering cellular matrix. Nine purine nucleosides were simultaneously quantified in 293T cells, and their concentrations ranged by 4 orders of magnitude. Overall, the method presents high recovery rates over 90% for endogenous modified purine nucleosides in cultured cells, along with good precision, linearity, and LOD ranging from 0.30 fmol to 0.37 pmol per 5 × 105 cells. The developed UHPLC–MS/MS method holds potential for screening purine nucleosides as diagnostic and prognostic biomarkers and for quantifying purine epigenetic nucleosides post-cell metabolome analysis, thereby providing a valuable analytical tool for intracellular nucleoside quantification in future clinical research.

CAS / MDL: 1867-73-8
研究领域: 分析化学 · 生物化学 · 分子生物学 · 癌症研究 · 代谢组学
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Biomed Research International · 2021 · IF 3.411

UPLC-ESI-MS/MS Analysis and Evaluation of Antioxidant Activity of Total Flavonoid Extract from Paeonia lactiflora Seed Peel and Optimization by Response Surface Methodology (RSM)

Guiqin Shi,Jiaxin Shen,Tao Wei,Fei Ren,Famou Guo,Yuan Zhou

In this study, the ultrasound-assisted extraction (UAE) of flavonoid from Paeonia lactiflora seed peel was optimized by response surface methodology (RSM). Single-factor experiments and a three-factor three-level Box-Behnken design (BBD) were performed to explore the effects of the following parameters on flavonoid extraction: ethanol concentration (), liquid-solid ratio (), and ultrasonic time (). The results showed that the optimal flavonoid yield (10.9045 mg RE/g) was as follows: ethanol concentration 62.93%, ultrasonic time 64.56 min, and liquid-solid ratio 24.86 mL/g. The optimized extract of P. lactiflora seed shell was further analyzed by UPLC-ESI-MS/MS, and 20 main flavonoids were identified and quantified, among which protocatechuic acid, vanillic acid, 4-hydroxybenzoic acid, and 3,4-dihydroxybenzaldehyde had the highest content. Furthermore, the results of the antioxidant test showed that the P. lactiflora seed peel extract obtained under optimized UAE conditions exhibited good antioxidant activity. The experimental results showed that ultrasound-assisted extraction was a fast, efficient, and simple method for extracting active ingredients from P. lactiflora seed peel, thereby making this byproduct a promising source of compounds in food and healthcare sectors.

研究领域: 药学 · 分析化学 · 食品科学 · 植物科学
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