RSC Advances
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2015
·Vol. 5
·期 60
·48885-48892
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IF 3.84
Hongkai Xie,Wenhua Ji,Dahui Liu,Wei Liu,Daijie Wang,Ruimin Lv,Xiao Wang
In this work, surface molecularly imprinted polymers with dummy templates were developed as the selective sorbents for preparation of dencichine from the extract of Panax notoginseng for the first time. The polymers were characterized by scanning electron microscopy and Fourier transform infrared spectroscopy. The performances of molecularly imprinted and non-imprinted polymers were evaluated, which included selective recognition, adsorption isotherms and adsorption kinetics. Optimization of various parameters affecting molecularly imprinted solid phase extraction, such as sample loading pH and flow rate, the composition and volume of the eluting solvent and the composition and volume of the washing solvent were investigated. Compared with NISPE, MISPE displayed improved specific adsorption performance. Dencichine with a purity of 98.7% was obtained from the aqueous extract of Panax notoginseng with the average recovery of 83.7% (n = 3).
研究领域:
药物化学
·
分析化学
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DOI
高影响因子
JOURNAL OF CHROMATOGRAPHY A
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2022
·
IF 4.601
Xiaoya Fu,Xia Wang,Zhining Xia,Yike Huang
To ensure drug safety, the quality monitoring of genotoxic impurities (GTIs) which have very trace content in medicine is important. Therefore, it should be established an efficient sample pretreatment method to extract GTIs to achieve specific enrichment. In this work, dummy template molecular imprinting technology (DMIT) was used as dummy template molecule (DTM) to substitute for the target molecule (TM) for established the pretreatment of the sample containing aromatic amine GTIs. A novel strategy for screening out DTM by calculation of computer simulation is established, where the binding energy between the template and functional monomer has the relatively lowest value (-9.60 kcal/mol). Then dummy template molecular imprinted polymer (DMIP) was prepared by bulk polymerization according to the molar ratio of template molecule-functional monomer-crosslinker = 1:4:8, the prepared DMIP exhibited the highest adsorption ( Q = 8.6 mg/g) and good blotting effect (IF = 1.3) and can simultaneously adsorb three aromatic amine GTIs. The optimal adsorption conditions were obtained by conditional optimization of solid phase extraction (SPE). The solution of pH 7 was chosen as the loading condition, and methanol/acetic acid (90:10, v/v) was chosen as the elution condition. Finally, we determined 2, 6-dichloroaniline in diclofenac sodium at a 5 ppm level and p-toluidine as the TMs in torasemide sample at 10 ppm by using DMIT-based solid phase extraction and analysis by HPLC, it satisfied the quality control of GTIs in pharmaceutics. DMIT by this strategy has great potential in the sample preparation of GTIs.
研究领域:
药学
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分析化学
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药物安全性评价
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DOI
PubMed
高影响因子
ANALYST
·
2013
·Vol. 138
·期 11
·3287-3296
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IF 3.969
Deli Xiao,Pierre Dramou,Nanqian Xiong,Hua He,Danhua Yuan,Hao Dai,Hui Li,Xiaomei He,Jun Peng,Nan Li
Fluoroquinolones (FQs) have emerged as one of the most important class of antibiotics. Due to their low concentration in bio-matrix samples which contain a lot of interfering substances, the efficient solid phase extraction and accurate determination of FQs remain a challenge. In this paper, a new strategy for the isolation and enrichment of FQs from egg samples was obtained by molecularly imprinted polymers on the surface of magnetic carbon nanotubes (MCNTs@MIP), which not only can be collected and separated rapidly by an external magnetic field, but also have a high specific surface area, outstanding mechanical properties and specific recognition for FQs. MCNTs@MIP were prepared using ofloxacin as a pseudo template, methacrylic acid as a functional monomer, and ethylene glycol dimethacrylate as a cross-linker. The characteristics of the MCNTs@MIP were assessed by transmission electron microscopy (TEM), multipoint Brunauer–Emmett–Teller (BET) analysis, vibrating sample magnetometry (VSM), X-ray diffraction (XRD) and Fourier transform infrared (FT-IR) spectroscopy. The results of the adsorption experiments not only demonstrated rapid dynamic adsorption but also showed a high selectivity toward FQs. An extraction method using MCNTs@MIP coupled with high performance liquid chromatography (HPLC) was developed for the determination of four FQs in egg samples. The recovery of four FQs ranged from 95.2% ± 3.2% to 100.7% ± 3.1% and the detection limits ranged from 0.25–0.40 ng g−1. The results demonstrate that the proposed method based on pseudo template MCNTs@MIP is a promising approach for the preconcentration, purification, and simultaneous analysis of four FQs in bio-matrix samples.
研究领域:
分析化学
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食品科学
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DOI
高影响因子
JOURNAL OF CHROMATOGRAPHY A
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2022
·
IF 4.601
Jianhua Xiong,Xiangting Wei,Xiantao Shen,Weiwei Zhu,Shaohua Yi,Chuixiu Huang
Determination of amphetamine-type drugs (ATSs) in urine and wastewater is a simplified approach for the widespread monitoring of ATSs abuse. To improve the sensitivity of the analytical methods, molecularly imprinted polymers (MIPs) based solid-phase extraction (SPE) pretreatment attracted great attention in this field. Generally, smaller particle sizes and more uniform morphology of the MIPs could provide higher detection sensitivity. Our previous works showed reflux precipitation polymerization (RPP) is a method for synthesizing monodispersed MIPs with small particle size. However, synthesis of uniform spherical MIPs towards a group of targets has never been reported. Therefore, in the present work, MIPs towards a group of ATSs were synthesized via RPP with a pseudo template for the first time. After screening potential pseudo-templates, N-methylphenylethylamine (MPEA) was selected as the optimal pseudo-template. MPEA-MIPs were characterized by scanning electron microscope (SEM), FT-IR spectroscopy and X-ray photoelectron spectroscopy (XPS) spectra. Adsorption isotherms, adsorption kinetics and selectivity were evaluated, and the experimental results indicated that the MPEA-MIPs possessed good selectivity and adsorption property towards ATSs. After optimization of the MIP-SPE procedure, the MIP-SPE cartridges were then coupled with liquid chromatography and tandem mass spectrometry (LC-MS/MS) for determination of ATSs. The evaluation results showed that MIP-SPE-LC-MS/MS displayed good linearity (R 2 >0.991) in the linear range (1.0–50.0 µg/L for urine and 0.5–50.0 µg/L for wastewater), and low matrix effect (85–112%). The limit of detection (LOD) was 0.05 -0.29 µg/L, and the accuracy (85–115%) and repeatability (RSD ≤ 15%) were satisfactory at low, medium and high concentrations. To the best of our knowledge, this is the first time that dummy MIPs towards a group of ATSs were synthesized by RPP polymerization, which showed great potential for the detection of ATSs in urine and wastewater.
研究领域:
分析化学
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环境科学
·
毒理学
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产品关联
DOI
PubMed
高影响因子
ANALYTICAL LETTERS
·
2017
·
IF 1.15
Xiuping He,Jiangtao Wang,Xiaoqi Mei
A multitemplate molecularly imprinted polymer was synthesized using fragments similar to gonyautoxins 1 and 4 including 2,4,6-triaminopyrimidine, 4-hydroxy-2-butanone, and imidazole as dummy templates by bulk polymerization. Scanning electron microscopy and infrared spectroscopy showed a porous structure and the formation of organic groups in the imprinting process of the polymer. One millilitre of 0.1 mol L−1 acetic acid and 1 mL of 95% methanol were the optimized washing and eluting solutions during the molecularly imprinted solid-phase extraction. The adsorption capacity of the multitemplate molecularly imprinted polymer was lower than for the monotemplate molecularly imprinted polymer prepared in a previous study in seawater in which Alexandrium tamarense and Alexandrium minutum were cultivated. This result may due to the inappropriate combination of the dummy template fragments in the synthesis resulting in the unfitness of the imprinting sites for gonyautoxins 1 and 4. In general, it is inappropriate to use fragments with the similar parts to the analyte as the dummy templates. However, this work indicated the optimal molecularly imprinted polymer for the selective extraction of gonyautoxins 1 and 4.
研究领域:
环境科学
·
分析化学
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DOI
高影响因子
TALANTA
·
2017
·
IF 4.162
Ming Zhang,Juan He,Yanzheng Shen,Weiye He,Yuanyuan Li,Dongxin Zhao,Shusheng Zhang
A polymer-based adsorption medium with molecular recognition ability for homologs of pyrethroids was prepared by atom transfer radical polymer iration using a fragment imprinting technique. Phenyl ether-biphenyl eutectic was utilized as a pseudo-template molecule, and the adsorption medium prepared was evaluated by solid-phase extraction and gas chromatography. Selectivity of the medium for pyrethroids was evaluated using it as solid phase extraction packing by Gas Chromatography. The results demonstrated that the absorption amount of bifenthrin , fenpropathrin , permethrin, cypermethrin, fenvalerate , Dursban and pentachloronitrobenzene for molecularly imprinted polymers were 2.32, 2.12, 2.18, 2.20, 2.30, 1.30 and 1.40 mg g −1 , respectively, while the non-imprinted polymers were 1.20, 1.13, 1.25, 1.05, 1.20, 1.23 and 1.32 mg g −1 , respectively. The rebinding test based on the molecularly imprinted solid phase extraction column technique showed the recoveries of honey sample spiked with seven insecticides within 88.5–106.2%, with relative standard deviations of 2.38–5.63%. Finally, the method was successfully applied to the analysis of pyrethroids in a honey sample.
研究领域:
分析化学
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环境科学
·
农药残留检测
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产品关联
DOI
PubMed
高影响因子
危险品化学品经营许可证（带存储）