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MICROCHIMICA ACTA · 2015 ·Vol. 183 ·期 1 ·415-421 · IF 3.741

Magnetic porous carbon-based solid-phase extraction of carbamates prior to HPLC analysis

Liu Xingli,Wang Chun,Wu Qiuhua,Wang Zhi

Magnetic Fe 3 O 4 -doped porous carbon (MPC) was synthesized by using a metal-organic framework as a sacrificial template and iron salts as magnetic precursors. The textural properties of the MPC were characterized by scanning electron microscopy, transmission electron microscopy, X-ray diffraction, vibration sample magnetometry, and nitrogen absorption-desorption isotherms. The MPC possesses a high specific surface and is strongly magnetic. It was employed as an adsorbent for magnetic solid-phase extraction of four carbamates. The main parameters that affect extraction efficiency were investigated. The carbamates were analyzed by high performance liquid chromatography with ultraviolet detection at 208 nm. Under optimum conditions, good linearity was achieved for all analytes in the 1–100 ng g −1 concentration range, with correlation coefficients of > 0.9992. The limits of detection (at an S/N ratio of 3) are between 0.1 and 0.2 ng g −1 , and the recoveries of spiked samples ranged from 89.3 to 109.7 %. A magnetic porous carbon (MPC) was synthesized using metal-organic framework as sacrificial template and Fe salts as magnetic precursor. The MPC showed high specific surface area and good magnetic property. It was employed as magnetic solid-phase extraction adsorbent for the extraction of carbamates from apple sample.

研究领域: 分析化学 · 环境科学 · 食品安全 · 材料科学 · 色谱技术
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BIOMEDICAL CHROMATOGRAPHY · 2019 ·Vol. 34 ·期 2 ·e4763 · IF 1.748

Screening of the potentially active compounds from Polygonatum sibiricum using RAW264.7 cellular membranes coated magnetic beads fishing followed by HPLC analysis

Qing-ling Qi,Ya-Ming Yu,Cheng Tang

Target biomolecule-immobilized magnetic beads could be used as a powerful tool for screening active compounds present in natural products. Low damage rates of the target proteins, associated with the availability of diverse automated online approaches for analysis, make it a valuable tool for affinity studies. RAW264.7 cells (a kind of murine macrophage cell line) were used in this study. These cellular membranes were immobilized onto the surface of MBs and were used for screening the active compounds of Polygonatum sibiricum. Combining this technique with HPLC led to the identification of an active compound and its biological activity was confirmed. This is the first report establishing the use of RAW264.7 cellular membrane-coated magnetic bead fishing followed by HPLC analysis for screening active compounds from natural products.

研究领域: 药理学 · 分析化学 · 细胞生物学 · 天然产物研究
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MICROCHIMICA ACTA · 2019 ·Vol. 186 ·期 4 ·1-9 · IF 5.479

One-pot fabrication of magnetic porous Fe3C/MnO/graphitic carbon microspheres for dispersive solid-phase extraction of herbicides prior to their quantification by HPLC

Tong Yao,Liu Xueyan,Zhang Lei

Magnetic porous microspheres composed of Fe 3 C, MnO and graphitic carbon (Fe 3 C/MnO/GC) were prepared by a one-pot method. A polycondensate obtained from urea and formaldehyde served as the carbon source and was calcined in the presence of metallic iron and manganese to yield Fe 3 C/MnO/GC. The resultant hybrid has highly mesoporous architecture, large specific surface, graphitic structure and adequate saturation magnetism. It is shown to possess excellent pre-concentration ability for herbicides (monuron, chlortoluron, atrazine and terbutylhylazine). The sorbent can be easily separated and has a long service lifetime (>25 cycles). Under optimized conditions, the sorbent excels by good recoveries (78–120%), high enrichment factors (45–50) and good precision (RSDs ≤10.7%). The limits of detection are 0.01–0.10 μg L −1 for (spiked) water samples, 0.22–0.87 μg kg −1 for grape samples, and 0.18–0.74 μg kg −1 for potato samples. This work offers a new strategy for the construction of magnetic bimetallic heterostructured GC hybrids. Schematic presentation of magnetic porous Fe 3 C/MnO/graphitic carbon microspheres and their application for the enrichment of trace level herbicides prior to HPLC analysis.

研究领域: 材料科学 · 环境科学 · 分析化学
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Analytical Methods · 2018 ·Vol. 11 ·期 1 ·105-112 · IF 2.073

Amino-functionalized mesoporous silica nanospheres (MSN-NH2) as sorbent for extraction and concentration of synthetic dyes from foodstuffs prior to HPLC analysis

Peige Qin,Yixin Yang,Wenqi Li,Jing Zhang,Qian Zhou,Minghua Lu

In this work, amino-functionalized mesoporous silica nanospheres (MSN-NH2) were synthesized and demonstrated as useful sorbents of dispersive solid-phase extraction (dSPE) for extraction and preconcentration of synthetic dyes (tartrazine, amaranth, sunset yellow, allura red, and orange II) from foodstuffs prior to high-performance liquid chromatography (HPLC) analysis. The MSN-NH2 was characterized by transmission electron microscopy, Fourier-transform infrared spectroscopy, nitrogen adsorption and desorption isotherms, and elemental analysis. To achieve optimized extraction efficiency, several critical factors including amount of MSN-NH2, sample pH, adsorption time, adsorption temperature, desorption time, and desorption solvents, were systematically investigated. Under the optimized conditions, the enrichment factors were higher than 120. The limits of detection were found to be 0.10–0.30 ng mL−1. The method showed excellent linearity in the range of 0.45–1000.0 ng mL−1 with correlation coefficients (R2) ≥ 0.9951. The intra-day and inter-day precision (n = 5) were 1.72–3.64% and 1.45–4.52%. The recoveries at three concentration levels ranged from 82.7 to 116.3%. The proposed dSPE by using MSN-NH2 as sorbent coupled with HPLC was successfully applied to the analysis of synthetic dyes in real samples.

研究领域: 分析化学 · 食品安全 · 材料科学
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MOLECULES · 2015 ·Vol. 20 ·期 4 ·7309-7324 · IF 2.416

Synthesis, Anti-Tumor and Anti-Angiogenic Activity Evaluations of Asiatic Acid Amino Acid Derivatives

Yue Jing,Gang Wang,Ying Ge,Minjie Xu,Zhunan Gong

Fifteen semi-synthetic derivatives of asiatic acid (AA) have been synthesized and evaluated for their biological activities. The successful modification of these compounds at the C-2, C-3, C-23 and C-28 positions was confirmed using NMR, MS and IR spectra. Further, their anti-tumor effects were evaluatedin vitrousing different cancer cell lines (HeLa, HepG2, B16F10, SGC7901, A549, MCF7 and PC3), while their anti-angiogenic activities were evaluatedin vivousing a larval zebrafish model. Among the derivatives, compounds4–10showed more potent cytotoxic and anti-angiogenic effects than AA, while compounds11–17had significantly less effects. The new derivative10was also included in finished formulations to evaluate its stability using HPLC due to its potential topical use. The derivative10had markedly better anti-tumor activities than both AA and other derivatives, with similar stability as its parent compound AA.Keywords:asiatic acid;amino acid derivatives;anti-tumor activity;anti-angiogenic effect;stability;HPLC analysis

研究领域: 药理学 · 肿瘤学 · 药物化学
✓ 已验证 DOI PubMed 高影响因子
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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS · 2018 · IF 2.831

Determination of caffeoylquinic acid derivatives in Azolla imbricata by chitosan-based matrix solid-phase dispersion coupled with HPLC–PDA

Weilin Wu,Wenqi Qian,Haitian Hao,Yun kang,Yaqin Wang,Yuanrong Deng,Chengjie Ni,Jianming Huang,Weiyu Weng

Five main components of Azolla imbricata were isolated and identified as caffeoylquinic acid derivatives, four of which were isolated from this species for the first time. The five compounds exhibited strong antioxidant activities and were used as chemical markers for quantitative analysis. A chitosan-based matrix solid-phase dispersion (MSPD) extraction coupled with high-performance liquid chromatography (HPLC) was developed for the determination of the five analytes in A. imbricata. The optimal conditions for the chitosan-based MSPD extraction were as follows: low viscosity chitosan HL-1 as the dispersant, sample-to-dispersant mass ratio of 1:1, 10 mL of a methanol-sulfuric acid aqueous solution (0.2 M) (7:3, v/v) as the elution solvent, and a grinding time of 1 min. Compared with ultrasonic assisted extraction (UAE), the chitosan-based MSPD extraction exhibited higher extraction efficiency, consumed less solvent and time, and provided a cleaner extract. Compared with C 18 -based MSPD, the developed method was less expensive and more environmentally-friendly. The validated MSPD–HPLC method was efficient, reliable, and applicable to the quantification of caffeoylquinic acids in A. imbricata .

研究领域: 植物化学 · 分析化学 · 药用植物研究
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ACS Omega · 2021 · IF 3.512

Rapid and Accurate Screening of Lysine-Producing Edible Mushrooms via the Homocitrate Synthase Gene as a Universal Molecular Marker

Zili Song,Ruilin Zhao,Hongjiao Zhang,Penglin Wei,Landa Qi,Guocan Chen,Wen-Bing Yin,Wei Li

Edible mushrooms are important nutraceutical sources of foods and drugs, which can produce various nutritional ingredients including all essential amino acids. The method of rapid screening for the strains producing specific functional components is very indispensable. Homocitrate synthase is one of the key enzymes in the α-aminoadipate pathway for lysine biosynthesis and has preferable sequence conservation in Agaricales. Based on the blast of homocitrate synthase homologous genes of strains of Agaricales, we achieved combinations of degenerate primers as molecular markers to rapidly screen the lysine-producing edible mushrooms. The experimental results revealed that the consistency between PCR amplification and HPLC analysis attained 82 and 75% in strains of Agaricales and Polyporales, respectively. The finding showed that the molecular marker has higher universality for screening edible mushroom resources of Agaricales. This PCR-based approach shows excellent potential in evaluating and discriminating edible wild-grown mushrooms with high lysine content in Agaricales.

CAS / MDL: 103-72-0
研究领域: 真菌学 · 分子生物学 · 食品科学
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