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1.
Highly selective molecularly imprinted polymers on the surface of silica gels were prepared by a sol–gel process and used as solid‐phase extraction adsorbents for the specific recognition, enrichment and detection of cloxacilloic acid in cloxacillin. The obtained polymers were characterized by scanning electron microscopy, FTIR spectroscopy, nitrogen adsorption and desorption, elemental analysis and thermogravimetric analysis. The imprinted polymers not only possessed high adsorption capacity (6.5 μg/mg), but also exhibited fast adsorption kinetics (they adsorb 80% of the maximum amount within 20 min) and excellent selectivity (the imprinted factor was 3.6). A method using the imprinted polymers as solid‐phase extraction adsorbents coupled with high‐performance liquid chromatography was established with good specificity, linearity (r = 0.9962), precision (ranging from 0.5 to 6.7%), accuracy (ranging from 93.9 to 97.7%) and extraction recoveries (ranging from 78.8 to 89.8%). The limits of detection and quantification were 0.07 and 0.25 mg/g, respectively. This work could provide a promising method in the enrichment, extraction and detection of allergenic impurities in the manufacture, storage and application of cloxacillin.  相似文献   

2.
Dexamethasone‐imprinted polymers were fabricated by reversible addition–fragmentation chain transfer polymerization on the surface of magnetic nanoparticles under mild polymerization conditions, which exhibited a narrow polydispersity and high selectivity for dexamethasone extraction. The dexamethasone‐imprinted polymers were characterized by scanning electron microscopy, transmission electron microscope, Fourier transform infrared spectroscopy, X‐ray diffraction, energy dispersive spectrometry, and vibrating sample magnetometry. The adsorption performance was evaluated by static adsorption, kinetic adsorption and selectivity tests. The results confirmed the successful construction of an imprinted polymer layer on the surface of the magnetic nanoparticles, which benefits the characteristics of high adsorption capacity, fast mass transfer, specific molecular recognition, and simple magnetic separation. Combined with high‐performance liquid chromatography, molecularly imprinted polymers as magnetic extraction sorbents were used for the rapid and selective extraction and determination of dexamethasone in skincare cosmetic samples, with the accuracies of the spiked samples ranging from 93.8 to 97.6%. The relative standard deviations were less than 2.7%. The limit of detection and limit of quantification were 0.05 and 0.20 μg/mL, respectively. The developed method was simple, fast and highly selective and could be a promising method for dexamethasone monitoring in cosmetic products.  相似文献   

3.
Steroid hormones as endocrine disrupting compounds can interfere with the functioning of hormonal systems of organisms and thus affect the health and reproduction of humans and wildlife. Unfortunately, these types of harmful endocrine disrupting compounds have been found in a variety of environmental samples at very low concentrations. Therefore, a simple, fast, and efficient method for enrichment of water samples is needed. A molecularly imprinted solid‐phase extraction combined with high performance liquid chromatography coupled with diode array detection was developed for the determination of six steroid hormones, such as estrone, 17‐β‐estradiol, estriol, 17‐α‐ethinylestradiol, progesterone, and testosterone in water samples. The recoveries obtained in the proposed method were in the range of 78.7–101.3%. Matrix effect below 20% suggests that the quantitative and qualitative results of the analysis were not significantly affected by the matrix. The results show that molecularly imprinted polymers based on spherical silica gel had the potential to be a highly innovative and selective sorbent. The proposed method was proved to be applicable for molecularly imprinted solid‐phase extraction in selective and reliable extraction and enrichment of steroid hormones in environmental water samples.  相似文献   

4.
In this study, novel monodisperse restricted access media‐molecularly imprinted polymers were successfully prepared by surface initiated reversible addition‐fragmentation chain transfer polymerization using monodisperse crosslinked poly (glycidyl methacrylate‐co‐ethylene glycol dimethacrylate) microspheres as the carrier and acryloyl chloride‐modified β‐cyclodextrin as the hydrophilic functional monomer. The surface morphology, protein exclusion, and adsorption properties of the molecularly imprinted polymers were investigated. The results show that the material has excellent monodispersity and hydrophilicity, and simultaneously exhibit high adsorption capacity, fast binding kinetics, high selectivity, and significant thermal stability. The molecularly imprinted polymers as dispersive solid‐phase extraction adsorbent combined with reversed‐phase high‐performance liquid chromatography was used to selectively enrich, separate, and analyze trace 17β‐estradiol in milk samples. The recovery of 17β‐estradiol is 88–95% with relative standard deviation of <4%, and the limits of detection and quantification of this method are 2.08 and 9.29 µg/L, respectively. The novel restricted access media‐molecularly imprinted polymer adsorbents provide an effective method for the selective extraction and detection of 17β‐estradiol directly from complex samples.  相似文献   

5.
A novel molecularly imprinted polymers based on multiwalled carbon nanotubes synthesized by precipitate polymerization was applied as a selective sorbent for separation and determination of rhein (4,5-dihydroxyanthraquinone-2-carboxylic acid) from the root of kiwi fruit samples coupled with high performance liquid chromatography (HPLC). The molecularly imprinted polymers were prepared with methacrylic acid and 4-vinylpyridine as bifunctional monomers. The chemical structure of the molecularly imprinted polymers was characterized by Fourier transform infrared spectrometer. The equilibrium rebinding experiment and competitive adsorption experiment showed that these imprinted polymers exhibited good adsorption ability toward rhein. The Langmuir adsorption equilibrium constant, K(m) , and theoretical maximum adsorption capacity, Q(m) , were estimated to be 0.43 and 6.77 mg g(-1) , respectively. Compared with molecularly imprinted polymers prepared with methacrylic acid or 4-vinylpyridine solely, the molecularly imprinted polymers synthesized with bifunctional monomers showed enhanced molecular imprinting effect and higher adsorption capacity for the template rhein. The performances of the molecularly imprinted polymers utilized as solid phase extraction sorbent were investigated in detail. The molecularly imprinted polymers prepared by the method proposed in this work could successfully apply to extraction and determination of rhein from the root of kiwi fruit samples coupled with HPLC.  相似文献   

6.
Ginsenoside Rg1 is a valuable bioactive molecule but its high polarity and low concentration in complex mixtures makes it a challenge to separate Ginsenoside Rg1 from other saponins with similar structures, resulting in low extraction efficiency. The successful development of effective Rg1 molecularly imprinted polymers that exhibit high selectivity and adsorption may offer an improved method for the enrichment of active compounds. In this work, molecularly imprinted polymers were prepared with two different methods, precipitation polymerization or surface imprinted polymerization. Comparison of the adsorption abilities showed higher adsorption of the surface molecularly imprinted polymers prepared by surface imprinted polymerization, 46.80 mg/g, compared to the 27.74 mg/g observed for the molecularly imprinted polymers prepared by precipitation polymerization. Therefore, for higher adsorption of the highly polar Rg1, surface imprinted polymerization is a superior technique to make Rg1 molecularly imprinted polymers. The prepared surface molecularly imprinted polymers were tested as a solid‐phase extraction column to directionally enrich Rg1 and its analogues from ginseng tea and total ginseng extracts. The column with surface molecularly imprinted polymers showed higher enrichment efficiency and better selectivity than a C18 solid‐phase extraction column. Overall, a new, innovative method was developed to efficiently enrich high‐polarity bioactive molecules present at low concentrations in complex matrices.  相似文献   

7.
Five iridoid glycosides were prepared using molecularly imprinted solid‐phase extraction combined with preparative high‐performance liquid chromatography. Hydrophilic molecularly imprinted polymers were synthesized using α‐1‐allyl‐2‐N‐acetyl glucosamine, which introduced an abundance of hydrophilic groups into the polymers. Using molecularly imprinted solid‐phase extraction as the sample pretreatment procedure, five iridoid glycosides, gardenoside, geniposide, shanzhiside, geniposidic acid, and genipin‐1‐O‐gentiobioside, were selectively enriched from Gardenia fructus extracts. Preparative high‐performance liquid chromatography then provided iridoid glycosides with a purity >98%. The structures were elucidated by using nuclear magnetic resonance spectroscopy, optical rotation and melting point measurements, and mass spectrometry. The results demonstrate that molecularly imprinted solid‐phase extraction combined with preparative high‐performance liquid chromatography was an efficient, rapid, and economical method for the preparation of bioactive compounds from natural products.  相似文献   

8.
The preparation of molecularly imprinted core–shell magnetic nanoparticles and their subsequent use in the solid‐phase extraction of thiabendazole from citrus sample extracts is described. Molecularly imprinted core–shell magnetic nanoparticles were prepared by the precipitation copolymerization of the imprinting polymerization mixture on the surface of vinyl‐modified silica magnetic nanoparticles and were characterized by Fourier transform infrared spectroscopy and scanning electron microscopy. The obtained molecularly imprinted core–shell magnetic nanoparticles exhibited a high selectivity for thiabendazole and were easily collected and separated by an external magnetic field without additional centrifugation or filtration steps. Under optimum conditions, a magnetic molecularly imprinted solid‐phase extraction method was developed allowing the extraction of thiabendazole from citrus sample extracts and final determination by high‐performance liquid chromatography with fluorescence detection. The detection limit was 0.2 mg/kg, far lower than the maximum residue limit established within the European Union for thiabendazole in citrus samples.  相似文献   

9.
This research highlights the application of highly efficient molecularly imprinted solid‐phase extraction for the preconcentration and analysis of melamine in aquaculture feed samples. Melamine‐imprinted polymers were synthesized employing methacrylic acid and ethylene glycol dimethacrylate as functional monomer and cross‐linker, respectively. The characteristics of obtained polymers were evaluated by scanning electron microscopy, Fourier transform infrared spectroscopy and binding experiments. The imprinted polymers showed an excellent adsorption ability for melamine and were applied as special solid‐phase extraction sorbents for the selective cleanup of melamine. An off‐line molecularly imprinted solid‐phase extraction procedure was developed for the separation and enrichment of melamine from aquaculture feed samples prior to high‐performance liquid chromatography analysis. Optimum molecularly imprinted solid‐phase extraction conditions led to recoveries of the target in spiked feed samples in the range 84.6–96.6% and the relative standard deviation less than 3.38% (n = 3). The aquaculture feed sample was determined, and there was no melamine found. The results showed that the molecularly imprinted solid‐phase extraction protocols permitted the sensitive, uncomplicated and inexpensive separation and pre‐treatment of melamine in aquaculture feed samples.  相似文献   

10.
A novel and highly efficient approach to obtain magnetic molecularly imprinted polymers is described to detect avermectin in fish samples. The magnetic molecularly imprinted polymers were synthesized by surface imprinting polymerization using magnetic multiwalled carbon nanotubes as the support materials, atom transfer radical polymerization as the polymerization method, avermectin as template, acrylamide as functional monomer, and ethylene glycol dimethacrylate as crosslinker. The characteristics of the magnetic molecularly imprinted polymers were assessed by using transmission electron microscopy, Fourier transform infrared spectroscopy, X‐ray photoelectron spectroscopy, vibrating sample magnetometry, X‐ray diffraction, and thermogravimetric analysis. The binding characteristics of magnetic molecularly imprinted polymers were researched through isothermal adsorption experiment, kinetics adsorption experiment, and the selectivity experiment. Coupled with ultra high performance liquid chromatography and tandem mass spectrometry, the extraction conditions of the magnetic molecularly imprinted polymers as adsorbents for avermectin were investigated in detail. The recovery of avermectin was 84.2–97.0%, and the limit of detection was 0.075 μg/kg. Relative standard deviations of intra‐ and inter‐day precisions were in the range of 1.7–2.9% and 3.4–5.6%, respectively. The results demonstrated that the extraction method not only has high selectivity and accuracy, but also is convenient for the determination of avermectin in fish samples.  相似文献   

11.
Double‐templated molecularly imprinted polymers with specific recognition of three matrine‐type alkaloids were prepared using matrine and oxymatrine as the template molecules. An approach based on double‐templated molecularly imprinted solid‐phase extraction coupled with high‐performance liquid chromatography and tandem mass spectrometry was then developed to extract and purify matrine, oxymatrine, and sophocarpine from Sophora moorcroftiana in the Tibetan plateau herbs. The polymers were characterized by Fourier‐transform infrared spectroscopy and scanning electron microscopy. Their adsorption characteristics were evaluated using adsorption kinetics, isotherms, selectivity, and recycling experiments. This polymer exhibited excellent molecular recognition ability and good selectivity. The obtained polymers as adsorbent was further used for the determination of three matrine‐type alkaloids coupled to high‐performance liquid chromatography with tandem mass spectrometry, the recoveries of three matrines spiked at three concentration levels in samples were 73.25–98.42% (n = 5) with a relative standard deviation less than 6.82%. The limits of detection for the method were 9.23–15.42 μg/kg (S/N = 3). This proposed method was assessed to be an effective method for simultaneous extraction, isolation, and identification of matrine, oxymatrine, and sophocarpine from Sophora moorcroftiana.  相似文献   

12.
A novel l‐ phenylalanine molecularly imprinted solid‐phase extraction sorbent was synthesized by the combination of Pickering emulsion polymerization and ion‐pair dummy template imprinting. Compared to other polymerization methods, the molecularly imprinted polymers thus prepared exhibit a high specific surface, large pore diameter, and appropriate particle size. The key parameters for solid‐phase extraction were optimized, and the result indicated that the molecularly imprinted polymer thus prepared exhibits a good recovery of 98.9% for l‐ phenylalanine. Under the optimized conditions of the procedure, an analytical method for l‐ phenylalanine was well established. By comparing the performance of the molecularly imprinted polymer and a commercial reverse‐phase silica gel, the obtained molecularly imprinted polymer as an solid‐phase extraction sorbent is more suitable, exhibiting high precision (relative standard deviation 3.2%, n = 4) and a low limit of detection (60.0 ± 1.9 nmol·L?1) for the isolation of l‐ phenylalanine. Based on these results, the combination of the Pickering emulsion polymerization and ion‐pair dummy template imprinting is effective for preparing selective solid‐phase extraction sorbents for the separation of amino acids and organic acids from complex biological samples.  相似文献   

13.
A novel magnetic molecularly imprinted polymer adsorbing material was successfully synthesized to detect ribavirin in animal feedstuff. Molecularly imprinted polymer was prepared through surface polymerization by using ribavirin as template molecule, methyl methacrylate, and γ‐methacryloxypropyl trimethoxy silane functionalized magnetic mesoporous silica as bifunctional monomers, and ethylene diglycidyl ether as crosslinking agent. The prepared magnetic molecularly imprinted polymer was characterized by scanning electron microscopy and infrared spectroscopy. Static and dynamic adsorption experiments and selective adsorption analysis were performed to evaluate the adsorption and selectivity of magnetic molecularly imprinted polymer. Different experiments were conducted to optimize the magnetic solid‐phase extraction conditions. Under optimal experimental conditions, a magnetic molecularly imprinted solid‐phase extraction coupled with high‐performance liquid chromatography method was successfully developed for ribavirin detection. The established method achieved a satisfactory linear range of 0.20–50 mg/L (R> 0.99) and a low detection limit (0.081 mg/kg). An average recovery of 92–105% with relative standard deviation of <6.5% was obtained upon the application of the developed method to detect ribavirin in real feedstuff samples. Thus, established method can be used for the rapid and simple separation and detection of added ribavirin in feedstuff.  相似文献   

14.
Toward improving the selective adsorption performance of molecularly imprinted polymers in strong polar solvents, in this work, a new ionic liquid functional monomer, 1‐butyl‐3‐vinylimidazolium bromide, was used to synthesize sulfamethoxazole imprinted polymer in methanol. The resulting molecularly imprinted polymer was characterized by Fourier transform infrared spectra and scanning electron microscopy, and the rebinding mechanism of the molecularly imprinted polymer for sulfonamides was studied. A static equilibrium experiment revealed that the as‐obtained molecularly imprinted polymer had higher molecular recognition for sulfonamides (e.g., sulfamethoxazole, sulfamonomethoxine, and sulfadiazine) in methanol; however, its adsorption of interferent (e.g., diphenylamine, metronidazole, 2,4‐dichlorophenol, and m‐dihydroxybenzene) was quite low. 1H NMR spectroscopy indicated that the excellent recognition performance of the imprinted polymer was based primarily on hydrogen bond, electrostatic and π‐π interactions. Furthermore, the molecularly imprinted polymer can be employed as a solid phase extraction sorbent to effectively extract sulfamethoxazole from a mixed solution. Combined with high‐performance liquid chromatography analysis, a valid molecularly imprinted polymer‐solid phase extraction protocol was established for extraction and detection of trace sulfamethoxazole in spiked soil and sediment samples, and with a recovery that ranged from 93–107%, and a relative standard deviation of lower than 9.7%.  相似文献   

15.
We describe novel cinnamic acid polydopamine‐coated magnetic imprinted polymers for the simultaneous selective extraction of cinnamic acid, ferulic acid and caffeic acid from radix scrophulariae sample. The novel magnetic imprinted polymers were synthesized by surface imprinting polymerization using magnetic multi‐walled carbon nanotubes as the support material, cinnamic acid as the template and dopamine as the functional monomer. The magnetic imprinted polymers were characterized by transmission electron microscopy, scanning electron microscopy, Fourier transform infrared spectroscopy and vibrating sample magnetometry. The results revealed that the magnetic imprinted polymers had outstanding magnetic properties, high adsorption capacity, selectivity and fast kinetic binding toward cinnamic acid, ferulic acid and caffeic acid. Coupled with high‐performance liquid chromatography, the extraction conditions of the magnetic imprinted polymers as a magnetic solid‐phase extraction sorbent were investigated in detail. The proposed imprinted magnetic solid phase extraction procedure has been used for the purification and enrichment of cinnamic acid, ferulic acid and caffeic acid successfully from radix scrophulariae extraction sample with recoveries of 92.4–115.0% for cinnamic acid, 89.4–103.0% for ferulic acid and 86.6–96.0% for caffeic acid.  相似文献   

16.
A novel 17β‐estradiol molecularly imprinted polymer was grafted onto the surface of initiator‐immobilized silica by surface‐initiated atom transfer radical polymerization. The resulting molecularly imprinted polymer was characterized by elemental analysis and thermogravimetric analysis. The binding property of molecularly imprinted polymer for 17β‐estradiol was also studied with both static and dynamic methods. The results showed that the molecularly imprinted polymer possessed excellent recognition capacity for 17β‐estradiol (180.65 mg/g at 298 K), and also exhibited outstanding selectivity for 17β‐estradiol over the other competitive compounds (such as testosterone and progesterone). Then, the determination of trace 17β‐estradiol in beef samples was successfully developed by using molecularly imprinted polymer solid‐phase extraction coupled with high‐performance liquid chromatography. The limit of detection was 0.25 ng/mL, and the amount of 17β‐estradiol in beef samples was detected at 2.83 ng/g. This work proposed a sensitive, rapid, reliable, and convenient approach for the determination of trace 17β‐estradiol in complicated beef samples.  相似文献   

17.
Nano‐sized molecularly imprinted polymers for tiliroside were successfully prepared by a precipitation polymerization method. Acrylamide, ethylene glycol dimethacrylate, azobisisobutyronitrile, and acetonitrile/dimethyl sulfoxide were used as functional monomer, cross‐linker, initiator, and porogen, respectively. The structural features and morphological characterization of tiliroside‐imprinted polymers were characterized by Fourier transform infrared spectroscopy and scanning electron microscopy, respectively. The adsorption experiments indicated that the tiliroside‐imprinted polymers exhibited high selective recognition property to tiliroside. Scatchard analysis indicated that the homogeneous‐binding sites were formed in the polymers. The selectivity test revealed that the adsorption capacity and selectivity of polymers to tiliroside was significantly higher than that of rutin, astragalin, and kaempferol. Finally, the tiliroside‐imprinted polymers were employed as adsorbents in solid‐phase extraction for the extraction of tiliroside from the ethyl acetate extract of the flowers of Edgeworthia gardneri (wall.) Meisn. The results demonstrated that the extraction recoveries of tiliroside ranged from 69.3 to 73.5% by using tiliroside‐imprinted polymers coupled with solid‐phase extraction method. These results indicated that the tiliroside‐based molecularly imprinted solid‐phase extraction method was proven to be an effective technique for the separation and enrichment of tiliroside from natural medicines.  相似文献   

18.
Methyltriphenylphosphonium bromide/chalcone/formic acid, a green ternary deep eutectic solvent, was applied as a functional monomer and dummy template simultaneously in the synthesis of a new molecularly imprinted polymer. Ternary deep eutectic solvent based molecularly imprinted polymers are used as a solid‐phase extraction sorbent in the separation and purification of rutin and quercetin from Herba Artemisiae Scopariae combined with high‐performance liquid chromatography. Fourier transform infrared spectroscopy and field‐emission scanning electron microscopy were applied to characterize the deep eutectic solvent based molecularly imprinted polymers synthesized using different molar ratios of chalcone. The static and competitive adsorption tests were performed to examine the recognition ability of the molecularly imprinted polymers to rutin and quercetin. The ternary deep eutectic solvent consisting of formic acid/chalcone/methyltriphenylphosphonium bromide (1:0.05:0.5) had the best molecular recognition effect. After optimization of the washing solvents (methanol/water, 1:9) and eluting solvents (acetonitrile/acetic acid, 9:1), a reliable analytical method was developed for strong recognition towards rutin and quercetin in Herba Artemisiae Scopariae with satisfactory extraction recoveries (rutin: 92.48%, quercetin: 94.23%). Overall, the chalcone ternary deep eutectic solvent‐based molecularly imprinted polymer coupled with solid‐phase extraction is an effective method for the selective purification of multiple bioactive compounds in complex samples.  相似文献   

19.
A molecularly imprinted polymer has been synthesized to specifically extract adefovir, an antiviral drug, from serum and urine by dispersive solid‐phase extraction before high‐performance liquid chromatography with UV analysis. The imprinted polymers were prepared by bulk polymerization by a noncovalent imprinting method that involved the use of adefovir (template molecule) and functional monomer (methacrylic acid) complex prior to polymerization, ethylene glycol dimethacrylate as cross‐linker, and chloroform as porogen. Molecular recognition properties, binding capacity, and selectivity of the molecularly imprinted polymers were evaluated and the results show that the obtained polymers have high specific retention and enrichment for adefovir in aqueous medium. The new imprinted polymer was utilized as a molecular sorbent for the separation of adefovir from human serum and urine. The serum and urine extraction of adefovir by the molecularly imprinted polymer followed by high‐performance liquid chromatography showed a linear calibration curve in the range of 20–100 μg/L with excellent precisions (2.5 and 2.8% for 50 μg/L), respectively. The limit of detection and limit of quantization were determined in serum (7.62 and 15.1 μg/L), and urine (5.45 and 16 μg/L). The recoveries for serum and urine samples were found to be 88.2–93.5 and 84.3–90.2%, respectively.  相似文献   

20.
The development of a simple and effective method for the isolation and purification of sulfadiazine residues in food of animal origin is of great significance since it is a great danger to human health. An off‐line molecularly imprinted solid‐phase extraction with high‐performance liquid chromatography method was proposed for the selective pretreatment and determination of sulfadiazine in eggs, rapidly and effectively. The molecularly imprinted polymer was proved to have a homogeneous spherical structure and porous surface morphology with excellent adsorption capacity of 5258 μg/g for sulfadiazine. The newly established method showed a good linearity in the range of 0–200 μg/L, low limits of detection (0.06 μg/L), acceptable reproducibility (RSD, 2.60–5.03%, n = 3), and satisfactory relative recoveries (78.22–86.10%). It was demonstrated that the proposed molecularly imprinted solid‐phase extraction with high‐performance liquid chromatography method could be applied to determine sulfadiazine in eggs, which simplified the pretreatment procedure and improved the accuracy of the analysis process by reducing the loss of sulfadiazine in the fat‐removing procedure compared with traditional methods. Molecularly imprinted solid‐phase extraction with excellent selectivity and adsorption capacity is a simple, rapid, selective, and effective pretreatment method for the determination of sulfadiazine in egg samples.  相似文献   

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