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UPLC-QqQ/MS
ULTRASONICS SONOCHEMISTRY · 2025 · IF 9.7

Flavonoids from sour jujube leaves: Ultrasound-assisted extraction, UPLC-QQQ-MS/MS quantification, and ameliorative effect on DSS-induced ulcerative colitis in mice

Hongke Wei,Xiaomin Wang,Jiaqi Wang,Shijie Ren,Luis A.J. Mur,Dong Lu,Duo Cao

To valorize sour jujube ( Ziziphus acidojujuba ) leaves, this work focused on the extraction, quantification, and bioactivity assessment of flavonoids. First, ultrasound-assisted extraction (UAE) was employed to extract total flavonoids from sour jujube leaves (SJL-TF), with the procedure optimized through single-factor design and response surface methodology (RSM). SJL-TF yield reached 48.47 ± 0.36 mg/g under optimal circumstances, which included 61 % ethanol as extraction medium, an ultrasound power of 300 W, an extraction time of 33 min, and a liquid–solid ratio of 16 mL/g, showing higher extraction efficiency in comparison to the traditional Soxhlet extraction method. Scanning electron microscopy (SEM) analysis indicated that ultrasound treatment severely damaged the structural integrity of sour jujube leaves, which was more conducive to improving the SJL-TF yield. Then, polyamide resin chromatography was used to purify the crude SJL-TF extracts, increasing the SJL-TF purity by 3.2-fold to 74.58 ± 0.63 %. By developing and validating a UPLC-QQQ-MS/MS method, ten main flavonoids in SJL-TF extracts, including catechin, rutin, isoquercetin, narirutin, nicotiflorin, quercitrin, phlorizin, luteolin, quercetin, and apigenin, were successfully detected concurrently for quality control purposes. Furthermore, the purified SJL-TF showed a strong ameliorative effect on dextran sulfate sodium (DSS)-induced ulcerative colitis (UC) in mice, as evidenced by significant mitigation of colonic inflammation and pathological damage. Thus, this work will contribute to improving the application of sour jujube leaves, especially in the pharmaceutical sector.

CAS / MDL: 21668-81-5
研究领域: 药理学 · 分析化学 · 植物化学
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INTERNATIONAL JOURNAL OF BIOLOGICAL MACROMOLECULES · 2024 · IF 7.7

Monosaccharide composition and glycosidic linkages analysis by ultra high performance liquid chromatography-triple quadrupole tandem mass spectrometry—Case study of plant polysaccharides

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.

CAS / MDL: 631-61-8 67-68-5
研究领域: 分析化学 · 植物学 · 生物化学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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Food Analytical Methods · 2025 · IF 3

Targeted LC–MS/MS Analysis of 11 Ranunculaceae Phytotoxins in Honey: Method Development, Validation, and Application to Real Samples

Lin Congcong,Zhu Xuena,Liu Rui,Zhang Li,Yu Tingting,Lu Qun

The consumption of honey contaminated with phytotoxins, particularly from Ranunculaceae plants, is a global public health concern due to their widespread distribution and diverse toxic compounds. This study developed a UPLC-QQQ-MS method to simultaneously quantify 11 phytotoxins of Ranunculaceae family in honey. Analytical (mobile phase) and pre-treatment (extraction solvent and cleanup column) procedures were optimized, identifying Methanol–Water (added 0.1% formic acid and 5 mM ammonium formate), acetonitrile, and SCX column as optimal. Method validation demonstrated negligible matrix effects, good linearity (R 2  > 0.995), good recoveries (81.38–116.85%), and high precision (RSD ≤ 8.63%) for 25–500 ng/mL ranges. LODs and LOQs were 0.02–0.15 µg/kg and 0.07–0.50 µg/kg, respectively (excluding anemonin). Retrospective analysis of 50 honey samples detected magnoflorine, talatisamine, hypaconitine, senecionine, and protopine at positive rates of 2%, 2%, 2%, 8%, and 10%, respectively. Thus, this work provides important technical supports for the risk assessment of phytotoxins in honey.

CAS / MDL: 540-69-2 64-18-6
研究领域: 分析化学 · 食品安全 · 毒理学 · 植物化学
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Journal of Chemistry · 2022 · IF 3.241

Evaluation of Multicomponent Changes of Schisandra chinensis Fruits with Different Drying Process by UPLC-QQQ-MS-Based Targeted Metabolomics Analysis

Yan-hua Sheng,Rui Wang,Yi-kai Wang,Meng-meng Li,Fang-xin Liu,Xin Huang,Chang-bao Chen

Schisandra chinensis fruit is a famous tonic traditional Chinese medicine and healthy food. The chemical components of dried fruits may vary with the initial processing methods of fresh fruits. Therefore, in this study, the influence of drying was evaluated based on targeted metabolomics analysis. The ultrahigh performance liquid chromatography-triple quadrupole mass spectrometry (UPLC-QQQ-MS) was applied in determination of multicomponent including lignans, organic acids, and oligosaccharides. The fresh fruits of Schisandra chinensis were processed by natural drying in the sun, hot air drying and vacuum drying at different temperatures, and vacuum freeze drying, respectively. The contents of lignans, organic acids, and oligosaccharides in different fruit samples were quantified and statistically analyzed by partial least squares discriminant analysis (PLS-DA). The variation of totally 10 lignans, 5 organic acids, and 9 oligosaccharides with different drying process were compared. The results showed that the drying time of natural drying method was much longer than the other methods using instrument. For hot air and vacuum drying samples, most of lignans, organic acids, and oligosaccharides gradually decreased with the increase of temperature. And the appearance of fruit drying at higher temperature was dark red. At the same processing temperature, vacuum drying takes longer time than hot air drying. In addition, organic acid and oligosaccharide contents of vacuum freeze drying treated samples were higher than the other processed samples significantly. According to the targeted metabolomics analysis, the lignans, organic acids, and oligosaccharides markers were screened out for holistic quality evaluation of Schisandra chinensis fruits. In comprehensive consideration of multicomponent, drying time, fruit appearance and storage, and production feasibility, hot air drying at 50°C is more suitable for the process of Schisandra chinensis. The result is expected to provide a scientific basis for the selection of proper method for drying process of fresh Schisandra chinensis fruit.

研究领域: 中药学 · 分析化学 · 食品科学
✓ 已验证 DOI 高影响因子
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ULTRASONICS SONOCHEMISTRY · 2025 · IF 9.7

Phenolics from Chaenomeles speciosa leaves: Ionic liquid-based ultrasound-assisted extraction, adsorptive purification, UPLC–QqQ–MS/MS quantification, and bioactivity assessment

Mengyang Hou,Chengyuan Lin,Lin Zhu,Zhaoxiang Bian

This study aimed to enhance the valorization of Chaenomeles speciosa leaves as a sustainable source of bioactive phenolics. An innovative ionic liquid-based ultrasound-assisted extraction (IL-UAE) method was developed for extracting phenolic compounds. Among 10 structurally diverse ILs, [BMIM]Br demonstrated superior extraction performance. Using a combination of single-factor design and response surface methodology (RSM), the optimal parameters for IL-UAE were determined to be the [BMIM]Br concentration of 1.33 mol/L, ultrasonic power of 380 W, extraction time of 10 min, and liquid-to-solid ratio of 22 mL/g. Under these conditions, the yield of C. speciosa leaves total phenolics (CSL-TP) was 78.14 ± 0.35 mg/g, which was substantially higher than those obtained via conventional heat reflux and UAE. After extraction, the microstructures of C. speciosa leaves were examined using scanning electron microscopy (SEM), which confirmed the effectiveness of IL-UAE. Subsequently, NKA-II resin column chromatography was developed to effectively purify crude CSL-TP extracts, guided by leakage and elution curve evaluations, yielding phenolic extracts with a purity of 75.40 % ± 1.93 %. A UPLC–QqQ–MS/MS method was developed for the quantitative analysis of nine major phenolics in purified CSL-TP extracts. Furthermore, bioactivity assessments demonstrated that the purified CSL-TP extracts efficiently scavenged radicals and effectively inhibited the proliferation of HCT-116 and HT-29 cell lines. These results highlight the potential of C. speciosa leaves as a valuable resource for the pharmaceutical and food industries, paving the way for the development of innovative therapeutic products and functional foods.

研究领域: 植物化学 · 分析化学 · 药理学
✓ 已验证 DOI PubMed 高影响因子
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RSC Advances · 2024 ·Vol. 14 ·期 35 ·25289-25300 · IF 3.9

Fabrication and characterization of TPGS-modified chlorogenic acid liposomes and its bioavailability in rats

Jian-jun Zhang,Qiu-shui Luo,Qing-qing Li,Qian Xu,Xiang Geng,Jian-hua Xiong

Chlorogenic acid (CGA), a polyphenol compound, exhibits excellent anti-oxidative, anti-hypoxic, antibacterial, antiviral, and anti-inflammatory activities, however the bioactivity of it has not been fully utilized in vivo due to its instability and low bioavailability. To address these issues, we prepared and characterized CGA-TPGS-LP, which is a TPGS-modified liposome loaded with CGA. The pharmacokinetics of CGA-TPGS-LP were studied in rats after oral administration. CGA-TPGS-LP was fabricated using a combination of thin film dispersion and ion-driven methods. The liposomes were observed to be uniformly small and spherical in shape. Their membranes were composed of lecithin, cholesterol, and TPGS lipophilic head with a TPGS hydrophilic tail chain coating on its surface. The loading efficiency and encapsulation efficiency were found to be 11.21% and 83.22%, respectively. The physicochemical characterisation demonstrated that the CGA was present in an amorphous form and retained its original structural state within the liposomal formulation. The stability of CGA was significantly improved by fabricating TPGS-LP. CGA-TPGS-LP exhibited good sustained-release properties in both simulated gastric and intestinal fluids. Following oral administration, ten metabolites were identified in rat plasma using UPLC-QTOF-MS. UPLC-QqQ-MS/MS quantitative analysis demonstrated that the oral bioavailability of CGA encapsulated in TPGS-modified liposomes was enhanced by 1.52 times. In addition, the three main metabolites of CGA had higher plasma concentrations and slower degradation rate. These results demonstrate that TPGS-modified liposomes could be a feasible strategy to further enhance the oral bioavailability of CGA, facilitating its clinical use.

CAS / MDL: 57-88-5 9002-96-4
研究领域: 药剂学 · 药理学 · 分析化学 · 药物递送系统
✓ 已验证 产品关联 DOI PubMed 高影响因子
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES · 2026 · IF 2.5

Comprehensive profiling and sensitive quantification of gangliosides in mouse brain based on boron-doped TiO2 composites coupled with UPLC-cIM-MS/UPLC-QQQ-MS/MS

Shuya Yang,Xianjun Zou,Shuhuan Chen,Yujie Li,Huma Javeria,Jehangir Khan,Zhenxia Du

Boron-doped TiO 2 enabled dual-mode enrichment of gangliosides from mouse brain. • Optimal conditions gave >98% elution efficiency and stable reuse over 6 adsorption–elution cycles. • UPLC-QQQ-MS/MS validation showed 2.5 enrichment factor, 44.5–116.9% recovery, and low LOD/LOQ. • UPLC-cIM-MS identified 33 gangliosides (8 subclasses), including 3 novel species. Gangliosides (GGs) play a crucial role in the development of the mammalian nervous system. However, due to their low content and significant matrix interference, the detection of these substance poses substantial challenges. In this study, considering that gangliosides contain a glycan headgroup with sialic acid residues, boron-doped titanium dioxide composites were prepared to enrich the GGs from mouse brain tissue by utilizing the specific affinity of boric acid for cis-diols of glycan and electrostatic attraction between TiO 2 and sialic acid ion. To optimize the extraction and elution parameters, a method of UPLC-QQQ-MS/MS was developed using the GGs standards, and then the extracts were analyzed by this method. The results showed that the boron-doped TiO 2 material significantly reduced matrix interference, with an average enrichment factor of 2.5 and recovery ranging from 44.5% to 116.9%. The limit of detection (LOD) was 0.5–20 μg/L, and the limit of quantification is 2–70 μg/L. To discover additional and novel GGs, the extracts underwent UPLC-cIM-MS to get the comprehensive profiles of GGs. Finally, 8 subclasses and 33 molecular structures of GGs were identified, and three new substances were discovered, which showed that boron-doped titanium dioxide composites coupled with LC-cIM-MS provide an effective strategy for the highly sensitive detection of GGs. Furthermore, this approach holds a great promise for expanding studies on GGs profiles in other complex biological samples.

✓ 已验证 DOI PubMed 高影响因子
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FOOD CHEMISTRY · 2023 · IF 8.8

One-step enrichment of phenolics from Chaenomeles speciosa (Sweet) Nakai fruit using macroporous resin: Adsorption/desorption characteristics, process optimization and UPLC-QqQ-MS/MS-based quantification

Mengyang Hou,Chengyuan Lin,Yanhua Ma,Jingchun Shi,Jie Liu,Lin Zhu,Zhaoxiang Bian

Chaenomeles speciosa (Sweet) Nakai fruit is a good source of phenolics with many health benefits. In this work, the enrichment of C. speciosa fruit total phenolics (CSFTP) using macroporous resins was studied. NKA-Ⅱ resin was selected for enriching CSFTP due to its highest adsorption/desorption quantity. Adsorption characteristics of CSFTP on NKA-Ⅱ resin exhibited a good fit with the Langmuir isotherm model and pseudo-second order kinetics model. This adsorption was spontaneous, exothermic, and entropy-decreasing through a physisorption mechanism. The breakthrough-elution curves were studied to optimize CSFTP enrichment conditions. One-step enrichment increased CSFTP content in the extracts from 26.51 % to 78.63 %, with a recovery of 81.03 %. A UPLC-QqQ-MS/MS method in multiple reaction monitoring (MRM) mode was established and validated for the simultaneous quantification of seven phenolic compounds. This study demonstrates the feasibility of industrial enrichment of CSFTP using NKA-Ⅱ resin and proposes a reliable method for quality control of CSFTP-rich products.

CAS / MDL: 154-23-4 99-50-3
✓ 已验证 产品关联 DOI PubMed 高影响因子
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FOOD AND CHEMICAL TOXICOLOGY · 2017 · IF 3.778

Identification of urine tauro-β-muricholic acid as a promising biomarker in Polygoni Multiflori Radix-induced hepatotoxicity by targeted metabolomics of bile acids

Dong-Sheng Zhao,Li-Long Jiang,Ya-Xi Fan,Lei-Chi Dong,Jiang Ma,Xin Dong,Xiao-Jun Xu,Ping Li,Hui-Jun Li

Polygoni Multiflori Radix (PMR) has been widely used as a tonic for centuries. However, hepatotoxicity cases linked to PMR have been frequently reported and appropriate biomarkers for clinical diagnosis are currently lacking. Here, an approach using UPLC-QqQ/MS-based targeted metabolomics of bile acids (BAs) complemented with biochemistry and histopathology was applied to characterize the development and recovery processes of PMR-induced hepatotoxicity in rats and to identify biomarkers. The expression of bile salt export pump (Bsep) and sodium taurocholate cotransporting polypeptide (Ntcp) were evaluated to investigate the underlying mechanism. Steatosis and inflammatory cell infiltration were observed in PMR-treated rats, which were accompanied by the elevation of serum biochemistry. The metabolic profiles of BAs were analyzed by Principal Component Analysis, hyodeoxycholic acid (HDCA) in serum and tauro-β-muricholic acid (TβMCA) in urine were identified as potential biomarkers for PMR-induced hepatotoxicity. The elevated expression of Bsep and decreased expression of Ntcp in the liver of PMRtreated rats indicated that hepatotoxicity was related to the disorders of BAs metabolism. Our study demonstrated that BAs may be used for clinical diagnosis of PMR-induced hepatotoxicity. Urine TβMCA was identified as a promising biomarker to facilitate the clinical monitoring of PMR-induced hepatotoxicity and may serve as potential therapeutic target.

CAS / MDL: 83-44-3 516-50-7
研究领域: 药理学 · 毒理学 · 代谢组学 · 肝病学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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