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CHEMICAL ENGINEERING JOURNAL · 2022 · IF 16.744

Facile construction of magnetic hydrophilic molecularly imprinted polymers with enhanced selectivity based on dynamic non-covalent bonds for detecting tetracycline

Yahan Cui,Jie Ding,Yu Su,Lan Ding

While a number of methods towards water-compatible molecularly imprinted polymers (MIPs) have been reported, new strategies affording simple preparation process and enhanced adsorption selectivity towards templates are needed to promote the further development of MIPs. Herein, we propose a novel method for preparing water-compatible MIPs (Cu-CMMIPs) with enhanced selectivity for tetracycline (TC) based on the dynamic physically cross-linking. The as-synthesized styrene-methacrylic acid copolymer was introduced as hydrophilic cross-linking functional monomers instead of conventional functional monomers and cross-linkers, thus eliminating the need of optimizing the cross-linkers/functional monomers ratio. The copper ions served as cross-linker, and in view of increased adsorption capacity and enhanced selectivity of the prepared MIPs, it was hypothesized that the introduction of copper ions would result in the strong interaction between the polymer network and TC. The imprinting process of TC is carried out by direct physical cross-linking of active groups of TC with functional groups of the polymeric network. The resultant Cu-CMMIPs exhibited excellent hydrophilicity, outstanding adsorption capacity and selectivity towards TC in water. Finally, the developed Cu-CMMIPs were applied as magnetic solid phase extraction adsorbents for the specific recognition of TC in environmental water combined with HPLC-DAD detection (LOD is 3.75 μg/L and the recoveries ranging from 91.2 % to 101.3 %). The proposed concept in this work for fabrication of MIPs with facile preparation process, enhanced selectivity and satisfactory hydrophilicity would inspire more ideas to implement in cost-effective adsorbents construction.

CAS / MDL: 57-68-1
研究领域: 材料科学 · 环境科学 · 分析化学
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Food Analytical Methods · 2021 ·Vol. 14 ·期 9 ·1895-1907 · IF 3.366

Development of an HPLC-DAD Method Combined with Chemometrics for Differentiating Geographical Origins of Chinese Red Wines on the Basis of Phenolic Compounds

Wu Qiao,Gu Hui-Wen,Yin Xiao-Li,Zhou Hui-Hui,Chang Hai-Yan,Shi Jie,Chen Ying,Yan Xiu-Fang,Liu Zhi

In this work, a high-performance liquid chromatography-diode array detection (HPLC-DAD) method combined with chemometrics was developed for differentiating geographical origins of Chinese red wines. Phenolic compounds were firstly detected and quantified by direct injection HPLC-DAD method in thirty red wines originated from two famous wine-growing regions in China. Given the high complexity of the wine samples and the co-elution problems during chromatographic separation, multivariate curve resolution-alternating least squares (MCR-ALS) was utilized to extract pure chromatographic and spectral profiles of each co-eluted compound. Quantification of phenolic compounds was thus achieved even in the presence of overlapping peaks and uncalibrated interferents. The quantitative data of the phenolic compounds in wines provided by the MCR-ALS algorithm were afterwards analyzed by unsupervised principal component analysis (PCA) and hierarchical cluster analysis (HCA) methods and supervised orthogonal partial least squares-discrimination analysis (OPLS-DA) method. Both PCA and HCA results showed that the thirty red wines from different geographical origins could be obviously distinguished, and the OPLS-DA could successfully predict the geographical origins of red wines. This study demonstrated that the HPLC-DAD method combined with chemometrics can be used as an effective tool for differentiating geographical origins of Chinese red wines on the basis of phenolic compounds.

研究领域: 食品科学 · 分析化学
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MICROCHEMICAL JOURNAL · 2024 · IF 4.9

Utilizing HPLC-DAD, multivariate analysis, molecular docking, and in vitro validation methods to investigate phenolic compounds with potential antidiabetic properties in Fraxinus mandshurica

Jianjin Guo,Chi-Tang Ho,Naisheng Bai

This comprehensive study utilized response surface methodology (RSM) to optimize extraction conditions for total flavonoids and phenols from F. mandshurica . Optimal conditions for flavonoids were 75 % ethanol, 63 °C, and 84 min, yielding 14.98 ± 0.13 mg/g. For phenols, it was 70 % ethanol, 66 °C, and 87 min, resulting in 26.04 ± 0.22 mg/g. UPLC-Q-TOF-MS/MS identified 68 constituents in F. mandshurica , categorized into groups. HPLC-DAD established a method for quantitative analysis of 12 target compounds. Geographical distribution analysis highlighted the northeast region as the main production area. Fingerprinting of 30 samples and multivariate analysis identified five active compounds. Hierarchical cluster analysis (HCA) showed differences in active compounds based on origin. In vitro antidiabetic evaluation demonstrated α-glucosidase inhibitory effects. Molecular docking studies were conducted between 12 active compounds and the antidiabetic-related protein 8A27. Esculetin had the highest binding affinity. The study examined extraction methods, analyzed samples, and explored antidiabetic effects, providing data support and insights for F. mandshurica as a natural industrial product and for extracts and active compounds as antidiabetic sources.

研究领域: 药理学 · 植物化学 · 生物信息学
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TALANTA · 2024 · IF 5.6

Dispersive liquid-liquid microextraction based on temperature-responsive supramolecular solvent followed by HPLC-DAD for the determination of pyrethroid pesticides in tobacco samples

Shurong Chen,Min Zhu,Ying Wang,Jinru Ding,Mingji Tan,Jindou Zhao,Jiahan Xie,Zhibing Wang

A novel temperature-responsive supramolecular solvent was prepared with cetyltributylphosphonium tetrafluoroborate and sodium citrate. It served as the extraction solvent of dispersive liquid-liquid microextraction for the extraction and enrichment of pyrethroids in tobacco samples. In this study, the preparation of the temperature-responsive supramolecular solvent and the extraction of the target analytes were integrated into one step, which simplified the experimental process. Due to the low melting point of the prepared supramolecular solvent, the traditional liquid-liquid separation can be converted to solid-liquid separation at low temperatures. This conversion facilitates precise collection of the supramolecular solvent and reduces the loss of target analytes. The composition, structure, physicochemical properties, and micromorphology of the supramolecular solvent were characterized. The formation and extraction mechanism of supramolecular solvent were explored, and the extraction conditions were optimized. The results indicated that good linearity of target analytes ( R 2  > 0.9998) was obtained within the linear range. The limits of detection and quantification for the five pyrethroids were in the range of 0.25–0.50 μg L −1 and 0.85–1.65 μg L −1 , respectively. The present method can be used for the analysis of pyrethroid pesticide residues in tobacco samples.

CAS / MDL: 68359-37-5 52645-53-1
研究领域: 分析化学 · 环境科学
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TALANTA · 2014 · IF 3.511

Magnetic solid-phase extraction based on methylcellulose coated-Fe3O4–SiO2–phenyl for HPLC–DAD analysis of sildenafil and its metabolite in biological samples

Minqiong Tang,Qing Wang,Ming Jiang,Li Xu,Zhi-Guo Shi,Ting Zhang,Yan Liu

In the present study, magnetic nanoparticles (MNPs) with phenyl functionalized core and a hydrophilic methylcellulose coating were synthesized. The functionalized MNPs showed excellent dispersibility in aqueous solution and they were applied to magnetic solid phase extraction (MSPE) of sildenafil and its metabolite, desmethyl sildenafil, from human urine and plasma samples followed by high performance liquid chromatographic analysis. The factors that may influence the extraction, including the amount of MNPs, pH and salt concentration of sample solution, extraction and desorption time, and the volume of desorption solvent, were investigated in detail. Under the optimum MSPE conditions, the developed method showed satisfactory reproducibility with intra-day and inter-day relative standard deviations less than 8.2% and low limits of detection of 0.41–0.96   ng   mL −1 from urine and plasma samples. The proposed material possessed good water compatibility and demonstrated excellent applicability for biological samples.

研究领域: 分析化学 · 药学
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Science China-Chemistry · 2018 ·Vol. 61 ·期 6 ·739-749 · IF 4.448

Simultaneous and interference-free determination of eleven non-steroidal anti-inflammatory drugs illegally added into Chinese patent drugs using chemometrics-assisted HPLC-DAD strategy

Wang Tong,Wu Hai-Long,Xie Li-Xia,Liu Zhi,Long Wan-Jun,Cheng Li,Ding Yu-Jie,Yu Ru-Qin

In this work, a smart strategy that combines three-way high performance liquid chromatography-diode array detection (HPLCDAD) data with second-order calibration method based on alternating trilinear decomposition (ATLD) algorithm was proposed for simultaneous determination of eleven non-steroidal anti-inflammatory drugs (NSAIDs) illegally added into Chinese patent drugs and health products. All target analytes were rapidly eluted out within 14.5 min under a simple gradient elution. With the aid of the prominent “second-order advantage” of the ATLD algorithm, three HPLC problems, i.e. peak overlaps, unknown interferences and baseline drift, could be mathematically calibrated, and pure signals of target analytes could be extracted out from heavy-interference but information-rich HPLC-DAD data. The average spiked recoveries for all target analytes were in the range of 95.9%–106.4% with standard deviations lower than 7.5%. Validation parameters including sensitivity (SEN), selectivity (SEL), limit of detection (LOD), limit of quantitation (LOQ) and precisions of intra-day and inter-day were calculated to validate the accuracy of the proposed method, quantitative results were further confirmed by the classic HPLC method, which proved that chemometrics-assisted HPLC-DAD analytical strategy was highly efficient, accurate and green for drug-abuse monitoring of NSAIDs in Chinese patent drugs and health products.

研究领域: 分析化学 · 药物分析 · 食品安全
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JOURNAL OF PHARMACOLOGICAL SCIENCES · 2015 · IF 2.36

Identification of schisandrin as a vascular endothelium protective component in YiQiFuMai Powder Injection using HUVECs binding and HPLC-DAD-Q-TOF-MS/MS analysis

Fang Li,Yi-Sha Tan,Hong-Lin Chen,Yan Yan,Ke-Feng Zhai,Da-Peng Li,Jun-Ping Kou,Bo-Yang Yu

YiQiFuMai Powder Injection (YQFM) is a re-developed preparation based on the well-known traditional Chinese medicine formula Sheng-mai-san. It has been widely used for the treatment of cardiovascular disease with definite clinical efficacy in China, but its bioactive molecules remain obscure. In this study, an effective method has been employed as a tool for screening active components in YQFM, using human umbilical vein endothelial cells (HUVECs) extraction and liquid chromatography coupled with electrospray ionization quadrupole time-of-flight tandem mass spectrometry (Q-TOF MS/MS). Nine compounds, which could interact with HUVECs, were identified as ginsenosides Rb1, Rc, Rb2, Rd, 20(S)-Rg3, 20(R)-Rg3, Rk1/Rg5 and schisandrin by comparing with reference substances or literature. In vitro assays showed that schisandrin at concentrations of 10–100 μM protected HUVECs from hypoxia/reoxygenation (H/R) injury, increased cell viability, nitric oxide (NO) content and decreased lactate dehydrogenase (LDH) leakage, malonaldehyde (MDA) content and ROS generation. Moreover, schisandrin pretreatment inhibited cell apoptosis, as evidenced by inhibiting activation of caspase-3 and increasing the Bcl-2/Bax ratio. These data indicate that HUVECs biospecific extraction coupled with HPLC-ESI-Q-TOF-MS/MS analysis is a reliable method for screening potential bioactive components from traditional Chinese medicines. Meanwhile, the vascular endothelium protective property of schisandrin might be beneficial for the treatment of cardiovascular disease.

CAS / MDL: 64-18-6
研究领域: 药理学 · 心血管科学 · 中药学
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Phytochemistry Letters · 2024 · IF 1.3

Simultaneous characterization and quantification of 25 flavonoid compounds in Actinidia arguta Miq. leaves by HPLC-DAD and screening for their inhibitory activity on α‑glucosidase

Yu-Fei Hou,Lu Bai,Shao-Jing Liu,Sen Guo,Ya-Long Wang,Chi-Tang Ho,Nai-Sheng Bai

A. arguta leaves, as an important by-product during the ripening of A. arguta fruits, are usually discarded. It contains numerous flavonoid components. In the present research, a simple and reproducible HPLC-DAD method was established and verified for simultaneous identification and quantification analysis of 25 flavonoid components in A. arguta leaves. The findings indicated that the highest concentration of flavonoid compounds in A. arguta leaves was quercetin ( 2 ), with a content of 8.97 ± 0.09 mg/g. The content of flavonoids in samples from different cultivation bases was different, indicating that the varied flavonoid contents are possibly determined by geographical variance. This method can be used for the quality control of Actinidia arguta . The 25 flavonoids showed good α-glucosidase inhibitory activity with IC 50 values ranging from 0.35 to 4.15 mM, and the activity difference varied with the different structures. 2"- O -galloylhyperin ( 18 ) showed the best antihyperglycemic action (IC 50 = 0.35 ± 0.01 mM), followed by quercetin ( 2 , IC 50 = 0.38 ± 0.01 mM), quercetin 4′- O -galactoside ( 19 , IC 50 = 0.41 ± 0.01 mM), kaempferol ( 3 , IC 50 = 0.42 ± 0.01 mM), and kaempferol-3-rutinoside ( 6 , IC 50 = 0.53 ± 0.01 mM). Molecular docking analysis demonstrated that the interaction modes of these five stronger inhibitors with α-glucosidase were mainly hydrogen bonding and hydrophobic interaction. The results showed that compounds with different structural skeletons interacted with different amino acid residues and exerted different degrees of α-glucosidase inhibition. Therefore, A. arguta leaves and their flavonoids may be beneficial against diabetes, and higher levels of flavonoids are considered to have greater potential for medicinal use.

研究领域: 药理学 · 分析化学 · 植物科学
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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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MICROCHEMICAL JOURNAL · 2020 · IF 3.594

Facile preparation of novel COFs functionalized magnetic core-shell structured nanocomposites and used for rapid detection of trace polycyclic aromatic hydrocarbons in food

Jian Chen,Na Li,Jianghua Liu,Fuping Zheng

A facile and rapid magnetic solid phase extraction (MSPE) based on magnetic covalent organic framework and coupled with high performance liquid chromatography diode array detection (HPLC-DAD) has been developed for detection of 11 kind of polycyclic aromatic hydrocarbons (PAHs) in food samples. In this paper, the novel magnetic core-shell structured (Fe 3 O 4 @COFs) nanocomposites were consisted with the magnetic Fe 3 O 4 nanoparticles (NPs) as a core, and 1,3,5-tris (4-aminophenyl) benzene (TAPB) and 2,5-dihydroxyterephthalaldehyde (DP) as two ligands for building shell outside of the core. These new nanocomposites were applied as superior adsorbent to enrich the PAHs due to their merits of large specific surface area, highly porosity and excellent thermal stability. The conditions that may affect the enrichment efficiency in MSPE process, including desorption solvent, amount of sorbent , extraction time, desorption time and desorption adsorption volume were investigated systematically. By combining MSPE with HPLC-DAD, an effective method for the detection of trace PAHs was successfully developed, which exhibited good linearity with R 2 ranging from 0.9954 to 0.9988, satisfactory recoveries in the range of 83.2–119.3%, and the relative standard deviations (RSD) was lower than 5.8%. In addition, the proposed MSPE-HPLC-DAD method was shown excellent ability to enrich trace PAHs effectively in food samples and potential application in extract other aromatic compounds .

研究领域: 分析化学 · 材料科学 · 环境科学 · 食品科学
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TALANTA · 2019 · IF 4.916

Target-based metabolomics for fast and sensitive quantification of eight small molecules in human urine using HPLC-DAD and chemometrics tools resolving of highly overlapping peaks

Xiao-Dong Sun,Hai-Long Wu,Zhi Liu,Yue Chen,Jun-Chen Chen,Li Cheng,Yu-Jie Ding,Ru-Qin Yu

Chemometrics multivariate calibration coupled with high performance liquid chromatography-diode array detection (HPLC-DAD) analytical strategy was applied for fast and sensitive quantification of the eight small molecules (uric acid, creatinine, tyrosine, homovanillic acid , hippuric acid, indole-3-acetic acid, tryptophan and 2-methylhippuric acid) in human urine. The objective of this work was to get the successful resolution of the complex matrix with minimum experimental time in the presence of highly overlapping peaks, of distortions in the time and baseline aspects among chromatograms, and of the presence of unknown and background interferences. All the analysis were based on a short C18 column with the chromatographic system operating in isocratic mode and all analytes can be successfully quantified within 6 min. The second-order HPLC-DAD data acquired were handled intelligently by two typical chemometrics tools including alternating trilinear decomposition (ATLD) and multivariate curve resolution-alternating least squares (MCR-ALS). Reasonable resolution and satisfactory quantification results were obtained regardless of the complex matrix interferences from the urine samples and the second-order advantage was fully exploited. With the validation by classic HPLC method, the proposed strategy could take extra advantages such as increased selectivity and sensitivity, shorter analysis time, undemanding elution conditions and sufficiency of lower limit of quantification benefit from multivariate calibration. The method was shown as a promising means for fast and sensitive determination of small molecules in human urine and also for fast diagnosis or surveillance in related diseases.

研究领域: 分析化学 · 医学检验 · 生物信息学
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TALANTA · 2020 · IF 5.339

Comparison of three chemometric methods for processing HPLC-DAD data with time shifts: Simultaneous determination of ten molecular targeted anti-tumor drugs in different biological samples

Yue-Yue Chang,Hai-Long Wu,Huan Fang,Tong Wang,Yang-Zi Ouyang,Xiao-Dong Sun,Gao-Yan Tong,Yu-Jie Ding,Ru-Qin Yu

Three intelligent chemometric multi-way calibration methods including alternating trilinear decomposition (ATLD), alternating trilinear decomposition assisted multivariate curve resolution (ATLD-MCR) and multivariate curve resolution-alternating least squares (MCR-ALS) combined with high performance liquid chromatography-diode array detection (HPLC-DAD) were used to quantify ten molecular targeted anti-tumor drugs in three complex biological matrices (plasma, urine and cell culture media matrices). All analytes can be successfully eluted in 6.5 min. In this experiment, various degrees of time shifts occurred in different samples. While slight time shifts exist in the chromatographic analysis , satisfactory results can be obtained by the three proposed methods. When the time shift was large (5.6 s), the average spiked recoveries obtained by ATLD analysis were in the range of 58.9%–116.5%, which was less than satisfactory. However, the average recoveries obtained by MCR-ALS and ATLD-MCR analysis were 89.8%–114.8% and 84.5%–106.1% respectively, and more satisfactory results were obtained. For further research, ATLD-MCR and MCR-ALS methods were compared, and the results were evaluated by statistical tests. Accuracies of concentrations obtained by them were considered to be no significant difference. In addition, compared with other methods currently published, the proposed chemometric methods combined with the HPLC-DAD can rapidly, simultaneously and accurately determine varieties of molecular targeted anti-tumor drugs in different complex biological matrices even in the presence of severe peak overlaps, severe time shifts, slight baseline drifts and different unknown background interferences.

研究领域: 分析化学 · 药物分析 · 化学计量学
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