首页 | 本学科首页   官方微博 | 高级检索  
相似文献
 共查询到20条相似文献,搜索用时 31 毫秒
1.
To obtain a highly selective material for the antibiotic chloramphenicol, which has several harmful side effects in humans, different molecularly imprinted polymers (MIPs) were prepared. In order to avoid a major traditional drawback associated with MIPs of residual template bleeding, molecules that are structurally related to chloramphenicol were used as templates for polymer synthesis. Chromatographic evaluation indicated that the employed template imparted a significant influence on the recognition properties of the corresponding polymer. A strong retention of chloramphenicol under nonpolar elution conditions (k = 68.03, IF = 17.72) and under aqueous elution conditions (k = 92.44, IF = 1.35) was achieved. After chromatographic evaluation, the MIP was utilized as the recognition sorbent in a solid-phase extraction to determine chloramphenicol using either an organic or aqueous washing solvent. Recoveries of nearly 100% from the chloramphenicol standard solution and nearly 90% from honey samples spiked with chloramphenicol were attained. Furthermore, the applicability of the MIP for sample cleanup was demonstrated.  相似文献   

2.
A selective, sensitive, rapid and reliable method based on molecularly imprinted polymers (MIPs) with dual templates to determine total content of parabens in cosmetics was developed. With methylparaben (MP) and propylparaben (PP) as dual-templates, methacrylic acid (MAA) as a functional monomer and tripropylene glycol diacrylate (TPGDA) as a cross-linker, MIPs film on a glassy carbon electrode was constructed as paraben sensor. At oxidation potential of 0.94 V (vs. SCE), the peak currents on the MIPs sensor were proportional to the concentration of parabens with square wave voltammetry. As the ratio of MP to PP in the MIPs was 1:1.25, the regression equations for four parabens were almost the same. The linear range was 20-100 μM for MP and EP, 5-100 μM for PP, and 5-80 μM for BP, with detection limit of 0.4 μM for MP and EP, 0.2 μM for the others. The total content of parabens could be calculated according to the average of these four regress equations. At least 10 times of structural analogs, such as p-hydroxybenzoic acid, p-aminobenzoic acid and phenol would not interfere with the determination of parabens. Nonanalogous coexistences such as vitamin C had no response on the sensor at all. Rapid response of the MIPs sensor was obtained within 1 min. MIPs sensor had been used to determine total content of parabens in cosmetic samples with recoveries between 98.7% and 101.8%. It reveals that the MIPs sensor with multi-templates has a potential to determine the total content of a group of homologous compounds.  相似文献   

3.
A variety of molecularly imprinted polymers (MIPs) against clozapine (CLZ) were synthesized and their recognition properties were compared with blank non-imprinted polymers. Methacrylic acid (MAA) was used as a functional monomer and Chloroform or tetrahydrofuran (THF) were applied as polymerization solvents. Chloroform as the solvent and MAA/CLZ ratio of 5 was selected as optimized polymerization condition. In Scatchard analysis of MIP-CLZ interactions, two classes of binding sites were found in MIP—high affinity (KD = 14.5 μM) and low affinity (KD = 322.5 μM) binding sites. The polymer was evaluated as a selective sorbent in molecularly imprinted solid-phase extraction (MISPE) of CLZ from human serum. The MISPE procedure was developed and optimized with a recovery of 88-102%. The intra- and inter-day precision values were less than 1.36% and 2.5%, respectively. The selectivity of MISPE for CLZ was studied in comparison with some drugs. These drugs could be present with CLZ, simultaneously in serum of patients. The data indicated that the imprinted polymer had a good selectivity and affinity for CLZ and could be used for selective extraction and analysis of CLZ in human serum.  相似文献   

4.
A novel and facile preparation method for layer-by-layer (LbL) self-assembled films incorporating quantum dots (QDs) and having intense photoluminescence (PL) from blue to red is presented. Functional sol-gel-derived glass layers prepared by the hydrolysis of 3-aminopropyltrimethoxysilane (APS) or 3-mercaptopropyltrimethoxysilane (MPS) have been used as a linkage between QD layers. Absorption, PL spectroscopy, transmission electron microscopy, and atomic force microscopy were employed for characterization, which revealed that the QDs in the prepared films had a nearly close-packed coverage and were not aggregated. The PL efficiencies of the QDs (CdTe or ZnSe, both are thioglycolic acid-stabilized) dispersed in the films were roughly half that of the initial colloidal solutions but reached 24% before a refractive index correction. The thickness of the red-emitting film with 10 CdTe QD layers was approximately 50 nm. The concentration of QDs in the film derived from the first absorption peak was approximately 0.01 M. Because the PL starts to show a red shift, the obtained concentration is practically the ultimate one in the glass matrix. The mercapto, amino, and carboxyl groups play important roles in LbL self-assembling processes.  相似文献   

5.
This work reports a comparative study of two automated flow-through fluorosensors for the determination of digoxin in serum samples: an immunosensor with an anti-digoxin polyclonal antibody as the reactive phase permanently immobilised on controlled-pore glass and a sensor with a selective reaction system based on a methacrylic molecularly imprinted polymer (MIP) synthesised by bulk polymerisation. The variables affecting the sensitivity and dynamic range of the sensors (e.g. the carrier and elution solutions, flow rates, pH and reagent concentrations) were optimized, and the binding characteristics of their reactive phases were compared in a competitive fluorescent assay. Digoxin was reproducibly determined by both sensors at the milligram per litre level (detection limit = 1.20 × 10−3 mg L−1 and RSD = 4–7% for the immunosensor; detection limit = 1.7 × 10−5 mg L−1 and RSD = 1–2% for the MIP sensor). No cross-reactivity with digoxin-related compounds was seen for either sensor at a digoxin/interferent ratio of 1:100. The lifetime of the immunosensor was about 50 immunoassays; its shelf life, when unused, is about 3 months. The lifetime of the MIP sensor was over 18 months. Both sensors were used to determine the digoxin concentration of human serum samples with satisfactory results.  相似文献   

6.
This is for the first time that application of complex nanostructure is reported as pH indicator in PVC matrix. This new optical pH sensor was constructed based on incorporation of ZnLI2 complex nanostructure in PVC matrix. The synthesized nanostructure ZnLI2 complex was characterized by SEM and XRD technique. The membrane solution was speared on the glass plate to provide thin film and the membrane surface morphology was investigated via field emission scanning microscope (FE‐SEM) technique. Central composite design (CCD) combined with desirability function (DF) was applied to find the best experimental composition of membrane providing the highest absorbance. These conditions were found in correspondence with 3 mg of pH indicator, 3 mg of ionic additive and 1.5 mg/mg of DBP/PVC weight ratio. Under optimum conditions, the proposed pH sensor has two linear working ranges of 4 ‐ 8 at 393 nm (R2 = 0.9897) and 5 ‐ 8 (R2 = 0.9982) at 570 nm with response time of 4 min. The pKa of proposed pH optical sensor was calculated through three methods that found to be 5.63. The present optical sensor shows stability after 2 months without any significant divergence in response properties (less than 5% RSD). Furthermore, current pH optode was exhibited good repeatability (RSD = 1.14%) as well as reproducibility (RSD = 4.06%). No significant variation was observed on sensor response with increasing the ionic strength in the range of 0.0–0.5 M of sodium chloride. All above features indicated that the proposed sensor can be successfully used for detection of pH in solutions with different ionic strength.  相似文献   

7.
Recently, molecular imprinted polymers (MIPs) were extensively used for separation and identification of specific molecules, replacing expensive and unstable biological receptors. Nonetheless, their application in electrochemical sensors has not been sufficiently explored. Here we report the use of a MIP as a specific receptor in a new highly sensitive tributyltin (TBT) electrochemical sensor. The sensor combines the specificity, pre-concentration capability and robustness of molecular imprinted polymer attached onto magnetic nanoparticles with the quantitative outputs of impedimetric measurements. The proposed device detects TBT in a concentration range of 5 pM to 5 μM with a low limit of detection (5.37 pM), which is lower than the one recommended for TBT in sea water by the US Environmental Protection Agency (EPA). We believe that this new electrochemical sensor can play an important role in the monitoring of the quality of sea and fresh waters worldwide.  相似文献   

8.
In this work, a novel and convenient strategy was developed to prepare molecularly imprinted polymers (MIPs) on the surface of graphene sheet. In this route, vinyl group functionalized graphene (GR/NVC) was first prepared by immobilizing 4-vinylcarbazole onto the surface of graphene via π–π interaction. The subsequent grafting copolymerization of methacrylic acid and ethylene glycol dimethacrylate in the presence of 4-nitrophenol (4-NP, template molecule) was carried out at GR/NVC surface, leading to the formation of GR/MIPs composite. The GR/MIPs composite was characterized by FTIR, fluorescence, TGA, SEM and AFM, and was used to fabricate electrochemical sensor for the detection of 4-NP. The electrochemical behavior of GR/MIPs sensor for 4-NP was investigated by cyclic voltammetry (CV) and differential pulse voltammetry (DPV). The effects of the preparation conditions, such as concentration of the NVC and template, the solution pH, and incubation time, were also optimized. Under optimized conditions, the DPV current response of GR/MIPs sensor was nearly 12 times than that of the GR/NIPs sensor. It also should be noted that as compared to traditional MIP, shorter response time and much higher current response were demonstrated. In addition, the GR/MIPs sensor could recognize 4-NP from its structural analogs, indicating the excellent selectivity of the GR/MIPs sensor. The peak current is linearly proportional to the concentration of 4-NP ranging from 0.01 μM to 100 μM and 200 μM to 1000 μM with a significantly low detection limit of 5 nM, a wider response range and lower detection limits as compared to most of the previously reported electrochemical sensors for 4-NP. Furthermore, the GR/MIPs sensor exhibits good stability with adequate reproducibility and has been successfully used to determine 4-NP in water samples.  相似文献   

9.
This work presents a comparison of convective interaction media (CIM) and controlled pore glass (CPG) as solid supports for immunoglobulin antibodies used in bioanalytical detection of allergens in foodstuffs. A flow-injection manifold with highly sensitive thermal lens spectrometric detection was used for this purpose. Using beta-lactoglobulin, a milk allergen, as a model analyte, CIM disc supports had a higher linear range (0.2–3.5 μg L−1), better reproducibility (intra-day RSD = 1%, inter-day RSD = 10%), lower consumption of reagents, and better immunocolumn stability (1 month, over 240 injections of substrate), while providing comparable LODs (0.1 μg L−1). Application of CIM discs as solid supports in immunocolumns for allergen detection enables fast and sensitive screening of allergens in foodstuffs with sample throughput of up to eight samples per hour.  相似文献   

10.
This paper reports a facile and general method for preparing an imprinted polymer thin shell with Mn-doped ZnS quantum dots (QDs) at the surface of silica nanoparticles by stepwise precipitation polymerization to form the highly-controllable core–shell nanoparticles (MIPs@SiO2–ZnS:Mn QDs) and sensitively recognize the target 2,4-dichlorophenol (2,4-DCP). Acrylamide (AM) and ethyl glycol dimethacrylate (EGDMA) were used as the functional monomer and the cross-linker, respectively. The MIPs@SiO2–ZnS:Mn QDs had a controllable shell thickness and a high density of effective recognition sites, and the thickness of uniform core–shell 2,4-DCP-imprinted nanoparticles was controlled by the total amounts of monomers. The MIPs@SiO2–ZnS:Mn QDs with a shell thickness of 45 nm exhibited the largest quenching efficiency to 2,4-DCP by using the spectrofluorometer. After the experimental conditions were optimized, a linear relationship was obtained covering the linear range of 1.0–84 μmol L−1 with a correlation coefficient of 0.9981 and the detection limit (3σ/k) was 0.15 μmol L−1. The feasibility of the developed method was successfully evaluated through the determination of 2,4-DCP in real samples. This study provides a general strategy to fabricate highly-controllable core–shell imprinted polymer-contained QDs with highly selective recognition ability.  相似文献   

11.
In this study, we have successfully prepared surface modified zinc oxide quantum dots (M-ZnO QDs) with ultra-stable fluorescence and excellent hydrophilicity through introducing (3-aminopropyl)triethoxysilane (APTES). The as-prepared M-ZnO QDs under the optimum condition presented strong yellow fluorescence emission under 355 nm excitation and showed satisfied reproducibility. Physical and chemical properties of the synthesized ZnO QDs were further studied by various characterization techniques. Transmission electron microscopy showed homogeneous distribution of spherical M-ZnO QDs with the average particle size of 4.03 nm. According to the characteristic that metal ions can quench fluorescence, M-ZnO QDs-based fluorescence sensor for the detection of Cu2+ in aqueous solution is developed in this work, which has the advantages of excellent selectivity, good sensitivity and a wide linear range. The limit of detection was 0.51 μM and the linear detection range was 1–200 μM for Cu2+ determination. The practicability of the fluorescent probe is further validated in the lake water and the satisfactory spiked recoveries of Cu2+ ranges from 99.1 % to 108.8 %. Besides, M-ZnO QDs displayed concentration inhibition effect and strain effect on the growth of fungi. Thus, the as-prepared M-ZnO QDs are demonstrated to be promising for Cu2+ determination and anti-fungal applications.  相似文献   

12.
This paper reports on the optimisation, characterisation, validation and applicability of gas chromatography coupled to triple quadrupole mass spectrometry in its tandem operation mode (GC-QqQ(MS/MS) for the quantification of polychlorinated dibenzo-p-dioxins and furans (PCDD/Fs, dioxins) and dioxin-like polychlorinated biphenyls (DL-PCBs) in environmental and food matrices. MS/MS parameters were selected to achieve the high sensitivity and selectivity required for the analysis of this type of compounds and samples. Good repeatability for areas (RSD = 1–10%, for PCDD/Fs and DL-PCBs) and for ion transition ratios (RSD = 0.3–10%, for PCDD/Fs, and 0.2–15%, for DL-PCBs) and low instrumental limits of detection, 0.07–0.75 pg μL−1 (for dioxins) and 0.05–0.63 pg μL−1 (for DL-PCBs), were obtained. A comparative study of the congener specific determination using both GC-QqQ(MS/MS) and gas chromatography-high resolution mass spectrometry (GC-HRMS) was also performed by analysing several fortified samples and certified reference materials (CRMs) with low (feed and foodstuffs), median (sewage sludge) and high (fly ash) toxic equivalency (TEQ) concentration levels, i.e. 0.60, 1.83, 72.9 and 3609 pg WHO-TEQ(PCDD/Fs) g−1. The agreement between the results obtained for the total TEQs (dioxins) on GC-QqQ(MS/MS) and GC-HRMS in all the investigated samples were within the range of ±4%, and that of DL-PCBs at concentration levels of 0.84 pg WHO-TEQs (DL-PCBs) g−1, in the case of feedstuffs, was 0.11%. Both instrumental methods have similar and comparable linearity, precision and accuracy. The GC-QqQ(MS/MS) sensitivity, lower than that of GC-HRMS, is good enough (iLODs in the down to low pg levels) to detect the normal concentrations of these compounds in food and environmental samples. These results make GC-QqQ(MS/MS) suitable for the quantitative analysis of dioxins and DL-PCBs and a real alternative tool to the reference sector HRMS instruments.  相似文献   

13.
Probe-donor integrated nanocomposites were developed from conjugating silica-coated Mn2+:ZnS quantum dots (QDs) with MoS2 QDs and photosensitive nitric oxide (NO) donors (Fe4S3(NO)7, RBS). Under excitation with near-infrared (NIR) light at 808 nm, the Mn2+:ZnS@SiO2/MoS2-RBS nanocomposites showed the dual-emissive two-photon excited photoluminescence (TPEPL) that induced RBS photolysis to release NO in situ. NO caused TPEPL quenching of Mn2+:ZnS QDs, but it produced almost no impact on the TPEPL of MoS2 QDs. Hence, the nanocomposites were developed as a novel QDs-based ratiometric TPEPL probe for real-time detection of NO release in situ. The ratiometric TPEPL intensity is nearly linear (R2 = 0.9901) with NO concentration in the range of 0.01∼0.8 μM, which corresponds to the range of NO release time (0∼15 min). The detection limit was calculated to be approximately 4 nM of NO. Experimental results confirmed that this novel ratiometric TPEPL probe possessed high selectivity and sensitivity for the detection of NO against potential competitors, and especially showed high detection performance for NIR-light triggered NO release in tumor intracellular microenvironments. These results would promote the development of versatile probe-donor integrated systems, also providing a facile and efficient strategy to real-time detect the highly controllable drug release in situ, especially in physiological microenvironments.  相似文献   

14.
Remote unattended sensor networks are increasingly sought after to monitor the drinking water distribution grid, industrial wastewater effluents, and even rivers and lakes. One of the biggest challenges for application of such sensors is the issue of in-field device calibration. With this challenge in mind, we report here the use of anodic stripping coulometry (ASC) as the basis of a calibration-free micro-fabricated electrochemical sensor (CF-MES) for heavy metal determinations. The sensor platform consisted of a photo-lithographically patterned gold working electrode on SiO2 substrate, which was housed within a custom stopped-flow thin-layer cell, with a total volume of 2–4 μL. The behavior of this platform was characterized by fluorescent particle microscopy and electrochemical studies utilizing Fe(CN)63−/4− as a model analyte. The average charge obtained for oxidation of 500 μM ferrocyanide after 60 s over a 10 month period was 176 μC, corresponding to a volume of 3.65 μL (RSD = 2.4%). The response of the platform to copper concentrations ranging from 50 to 7500 ppb was evaluated, and the ASC results showed a linear dependence of charge on copper concentrations with excellent reproducibility (RSD ≤ 2.5%) and accuracy for most concentrations (≤5–10% error). The platform was also used to determine copper and mercury mixtures, where the total metallic content was measurable with excellent reproducibility (RSD ≤ 4%) and accuracy (≤6% error).  相似文献   

15.
This work presents the potential application of organic-resistant screen-printed graphitic electrodes (SPGEs) for fuel analysis. The required analysis of the antioxidant 2,6-di-tert-butylphenol (2,6-DTBP) in biodiesel and jet fuel is demonstrated as a proof-of-concept. The screen-printing of graphite, Ag/AgCl and insulator inks on a polyester substrate (250 μm thickness) resulted in SPGEs highly compatible with liquid fuels. SPGEs were placed on a batch-injection analysis (BIA) cell, which was filled with a hydroethanolic solution containing 99% v/v ethanol and 0.1 mol L−1 HClO4 (electrolyte). An electronic micropipette was connected to the cell to perform injections (100 μL) of sample or standard solutions. Over 200 injections can be injected continuously without replacing electrolyte and SPGE strip. Amperometric detection (+1.1 V vs. Ag/AgCl) of 2,6-DTBP provided fast (around 8 s) and precise (RSD = 0.7%, n = 12) determinations using an external calibration curve. The method was applied for the analysis of biodiesel and aviation jet fuel samples and comparable results with liquid and gas chromatographic analyses, typically required for biodiesel and jet fuel samples, were obtained. Hence, these SPGE strips are completely compatible with organic samples and their combination with the BIA cell shows great promise for routine and portable analysis of fuels and other organic liquid samples without requiring sophisticated sample treatments.  相似文献   

16.
In this paper we report the synthesis of monolithic molecularly imprinted polymers (monolithic MIPs) for the chromatographic separation of Z-phenylalanine by “in situ” polymerisation. Four different functional monomers were used for the preparation and the columns were tested with a standard mobile phase of 1% acetic acid in acetonitrile. 4-Vinylpyridine has shown the best separation performance with a resolution factor R>1 and was chosen for a further improvement of the imprinted stationary phase, which leads to a resolution factor R=2.06. All monoliths investigated have surface areas of around 400 m2 g−1. The columns containing 4-vinylpyridine as functional monomer were characterised by frontal analysis and peak fitting method. These methods allow the determination of the adsorption isotherm which quantify the separation potential of the imprinted monoliths.  相似文献   

17.
A novel molecularly imprinted polymer based on graphene oxide was prepared as a solid‐phase extraction adsorbent for the selective adsorption and extraction of cyromazine from seawater samples. The obtained graphene oxide molecularly imprinted polymer and non‐imprinted polymer were nanoparticles and characterized by scanning electron microscopy. The imprinted polymer showed higher adsorption capacity and better selectivity than non‐imprinted polymer, and the maximum adsorption capacity was 14.5 mg/g. The optimal washing and elution solvents for molecularly imprinted solid phase extraction procedure were 2 mL of acetonitrile/water (80:20, v/v) and methanol/acetic acid (70:30, v/v), respectively. The recoveries of cyromazine in the spiked seawater samples were in the range of 90.3–104.1%, and the relative standard deviation was <5% (n = 3) under the optimal procedure and detection conditions. The limit of detection of the proposed method was 0.7 μg/L, and the limit of quantitation was 2.3 μg/L. Moreover, the imprinted polymer could keep high adsorption capacity for cyromazine after being reused six times at least. Finally, the synthesized graphene oxide molecularly imprinted polymer was successfully used as a satisfied sorbent for high selectivity separation and detection of cyromazine from seawater coupled with high‐performance liquid chromatography.  相似文献   

18.
Benzhydryl protection by diphenyldiazomethane of an alcohol in enantiomeric base-sensitive ribonolactones allows short efficient syntheses of 1,4-dideoxy-1,4-imino-d-lyxitol (DIL) and of 1,4-dideoxy-1,4-imino-l-lyxitol (LIL). DIL showed potent [Ki = 0.13 μM]—and LIL showed weak [Ki = 113 μM]—competitive inhibition of α-d-galactosidase. Both enantiomers N-benzyl-DIL [Ki = 64 μM] and N-benzyl-LIL [Ki = 13 μM] were moderate competitive inhibitors of naringinase, an α-l-rhamnosidase.  相似文献   

19.
Song  Wei  Chen  Yu  Xu  Juan  Yang  Xiao-Rong  Tian  Dan-Bi 《Journal of Solid State Electrochemistry》2010,14(10):1909-1914
Molecularly imprinted polymers (MIPs) have been applied as molecular recognition elements to chemical sensors. In this paper, we combined the use of MIPs and electropolymerization to produce a sensor which was capable of detecting dopamine (DA). The MIP electrode was obtained by electrocopolymerization of o-phenylenediamine and resorcinol in the presence of the template molecular DA. The MIP electrode exhibited a much higher current response compared with the non-imprinted electrode. The response of the imprinted sensor to DA was linearly proportional to its concentration over the range 5.0 × 10−7-4.0 × 10−5 M. The detection limit of DA is 0.13 μM (S/N = 3). Moreover, the proposed method could discriminate between DA and its analogs, such as ascorbic acid and uric acid. This method was successfully applied to the determination of DA in dopamine hydrochloride injection and healthy human blood serum. These results revealed that such a sensor fulfilled the selectivity, sensitivity, sped, and simplicity requirements for DA detection and provided possibilities of clinical application in physiological fields.  相似文献   

20.
A piezoelectric quartz crystal (PQC) sensor based on a molecularly imprinted polymer (MIP) has been developed for enantioselective and quantitative analysis of d-(+)-methamphetamine (d(+)-MA). The sensor was produced by bulk polymerization and the resulting MIP was then coated on the gold electrode of an AT-cut quartz crystal. Conditions such as volume of polymer coating, curing time, type of PQC, baseline solvent, pH, and buffer type were found to affect the sensor response and were therefore optimized. The PQC-MIP gave a stable response to different concentrations of d(+)-MA standard solutions (response time = 10 to 100 s) with good repeatability (RSD = 0.03 to 3.09%; n = 3), good reproducibility (RSD = 3.55%; n = 5), and good reversibility (RSD = 0.36%; n = 3). The linear range of the sensor covered five orders of magnitude of analyte concentration, ranging from 10−5 to 10−1 μg mL−1, and the limit of detection was calculated as 11.9 pg d(+)-MA mL−1 . The sensor had a highly enantioselective response to d(+)-MA compared with its response to l(−)-MA, racemic MA, and phentermine. The developed sensor was validated by applying it to human urine samples from drug-free individuals spiked with standard d(+)-MA and from a confirmed MA user. Use of the standard addition method (SAM) and samples spiked with d(+)-MA at levels ranging from 1 × 10−3 to 1 × 10−2 μg mL−1 showed recovery was good (95.3 to 110.9%).  相似文献   

设为首页 | 免责声明 | 关于勤云 | 加入收藏

Copyright©北京勤云科技发展有限公司  京ICP备09084417号