Poly glycidyl methacrylate‐co‐ethylene dimethacrylate porous monolith as a versatile platform for the development of separations and solid‐phase extractions in sequential injection analyzers
Abstract:We demonstrated that the porous structure and the reactivity of the epoxy group in the poly glycidyl methacrylate‐co‐ethylene dimethacrylate monolith can be a platform for the development of separation and extraction methods based on sequential injection analysis. The epoxy group was functionalized to produce monoliths affording complexing and ion exchange properties. Derivatization with iminodiacetate and sodium sulfite produced weak and strong cation exchangers, respectively. Derivatization with ethylenediam… Show more
“…The primary vibration of the sulfonate groups (the stretching of the S=O bond at 1375-1335 cm −1 ) does not appear in our polymers (Supporting Information Figure S2). From the cation exchange capacity of the sulfonated poly(GMA-co-EDMA), formerly estimated as 14 mg/g of Cu 2+ [18], and admitting a 1:1 exchange stoichiometry, we estimate the presence of 0.71 wt% of S. The low incorporation of S and N is consistent with a significant part of the epoxy groups buried in the polymer matrix. It is also consistent with the partial hydrolysis of the surface epoxy to form diols [23].…”
Section: Attenuated Total Reflectance Fourier Transform Infrared Specmentioning
confidence: 75%
“…Peters et al were the first to propose the mixture of 1-propanol, 1,4 butanediol, and water as a means to control the size of the pores over a broad range by just varying the ratio of 1-propanol to 1,4-butanediol [27]. By our experience with low-pressure sequential injection analyzers, the use of this porogenic F I G U R E 1 Scanning electron microscopy of the core of the polymer monoliths before and after the functionalizations with Na 2 SO 3 and IDA mixture offers poly(GMA-co-EDMA) columns with lower pressure drops than those synthesized in 1-dodecanol and cyclohexanol [18,28]. Darcy's equation computed the permeability of the columns from the back pressures measured at a flow rate of 500 µL/min of deionized water and ambient temperature.…”
Section: Scanning Electron Microscopymentioning
confidence: 99%
“…In that work, however, no chromatographic separations were demonstrated. Poly(GMA‐ co ‐EDMA) is a versatile monolithic platform to produce columns for the separation of proteins by ion‐exchange, reversed‐phase, and immobilized metal affinity chromatographic modes [11,18,19]. The most straightforward approach to produce ion exchange monolithic columns is the copolymerization of the crosslinker with an ionizable monomer, such as methacrylic acid [20] or 2‐acrylamide‐2‐methyl‐1‐propane sulfonic acid [21] (weak and strong cation exchangers, respectively).…”
We describe the synthesis of polymer monoliths inside polypropylene tubes from ink pens. These tubes are cheap, chemically stable, and resistant to pressure. UV-initiated grafting with 5 wt% benzophenone in methanol for 20 min activated the internal surface, thus enabling the covalent binding of ethylene glycol dimethacrylate, also via photografting. The pendant vinyl groups attached a poly(glycidyl methacrylate-co-ethylene glycol dimethacrylate) monolith prepared via photopolymerization. These tubes measured 100-110 mm long, with 2 mm of internal diameter. The parent monoliths were functionalized with Na 2 SO 3 or iminodiacetate to produce strong and weak cation exchangers, respectively. The columns exhibited permeabilities varying from 2.7 to 3.3 × 10 −13 m 2 , which enabled the separation of proteins at 500 µL/min and back pressures <2.8 MPa. Neither structure collapse nor monolith detachment occurred at flow rates as high as 2.0 mL/min, which produced back pressures between 6.9 and 9.0 MPa. The retention times of ovalbumin, ribonuclease A, cytochrome C, and lysozyme in salt gradient at pH 7.0 followed the order of increasing isoelectric points, confirming the cation exchange mechanism. Separation and determination of lysozyme in egg white proved the applicability of the columns to the analysis of complex samples.
“…The primary vibration of the sulfonate groups (the stretching of the S=O bond at 1375-1335 cm −1 ) does not appear in our polymers (Supporting Information Figure S2). From the cation exchange capacity of the sulfonated poly(GMA-co-EDMA), formerly estimated as 14 mg/g of Cu 2+ [18], and admitting a 1:1 exchange stoichiometry, we estimate the presence of 0.71 wt% of S. The low incorporation of S and N is consistent with a significant part of the epoxy groups buried in the polymer matrix. It is also consistent with the partial hydrolysis of the surface epoxy to form diols [23].…”
Section: Attenuated Total Reflectance Fourier Transform Infrared Specmentioning
confidence: 75%
“…Peters et al were the first to propose the mixture of 1-propanol, 1,4 butanediol, and water as a means to control the size of the pores over a broad range by just varying the ratio of 1-propanol to 1,4-butanediol [27]. By our experience with low-pressure sequential injection analyzers, the use of this porogenic F I G U R E 1 Scanning electron microscopy of the core of the polymer monoliths before and after the functionalizations with Na 2 SO 3 and IDA mixture offers poly(GMA-co-EDMA) columns with lower pressure drops than those synthesized in 1-dodecanol and cyclohexanol [18,28]. Darcy's equation computed the permeability of the columns from the back pressures measured at a flow rate of 500 µL/min of deionized water and ambient temperature.…”
Section: Scanning Electron Microscopymentioning
confidence: 99%
“…In that work, however, no chromatographic separations were demonstrated. Poly(GMA‐ co ‐EDMA) is a versatile monolithic platform to produce columns for the separation of proteins by ion‐exchange, reversed‐phase, and immobilized metal affinity chromatographic modes [11,18,19]. The most straightforward approach to produce ion exchange monolithic columns is the copolymerization of the crosslinker with an ionizable monomer, such as methacrylic acid [20] or 2‐acrylamide‐2‐methyl‐1‐propane sulfonic acid [21] (weak and strong cation exchangers, respectively).…”
We describe the synthesis of polymer monoliths inside polypropylene tubes from ink pens. These tubes are cheap, chemically stable, and resistant to pressure. UV-initiated grafting with 5 wt% benzophenone in methanol for 20 min activated the internal surface, thus enabling the covalent binding of ethylene glycol dimethacrylate, also via photografting. The pendant vinyl groups attached a poly(glycidyl methacrylate-co-ethylene glycol dimethacrylate) monolith prepared via photopolymerization. These tubes measured 100-110 mm long, with 2 mm of internal diameter. The parent monoliths were functionalized with Na 2 SO 3 or iminodiacetate to produce strong and weak cation exchangers, respectively. The columns exhibited permeabilities varying from 2.7 to 3.3 × 10 −13 m 2 , which enabled the separation of proteins at 500 µL/min and back pressures <2.8 MPa. Neither structure collapse nor monolith detachment occurred at flow rates as high as 2.0 mL/min, which produced back pressures between 6.9 and 9.0 MPa. The retention times of ovalbumin, ribonuclease A, cytochrome C, and lysozyme in salt gradient at pH 7.0 followed the order of increasing isoelectric points, confirming the cation exchange mechanism. Separation and determination of lysozyme in egg white proved the applicability of the columns to the analysis of complex samples.
“…The most frequently used organic monoliths in AMC are based on copolymers of glycidyl methacrylate (GMA) and ethylene glycol dimethacrylate (EDMA) [19,44,50,61–65]. GMA/EDMA monoliths can be readily synthesized and are commercially available under the trade name “convective interaction media” (CIM) [15,20,44].…”
Affinity monolith chromatography (AMC) is a liquid chromatographic technique that utilizes a monolithic support with a biological ligand or related binding agent to isolate, enrich, or detect a target analyte in a complex matrix. The target‐specific interaction exhibited by the binding agents makes AMC attractive for the separation or detection of a wide range of compounds. This article will review the basic principles of AMC and recent developments in this field. The supports used in AMC will be discussed, including organic, inorganic, hybrid, carbohydrate, and cryogel monoliths. Schemes for attaching binding agents to these monoliths will be examined as well, such as covalent immobilization, biospecific adsorption, entrapment, molecular imprinting, and coordination methods. An overview will then be given of binding agents that have recently been used in AMC, along with their applications. These applications will include bioaffinity chromatography, immunoaffinity chromatography, immobilized metal‐ion affinity chromatography, and dye‐ligand or biomimetic affinity chromatography. The use of AMC in chiral separations and biointeraction studies will also be discussed.
“…In liquid chromatography, the derivatization procedure can be performed either in pre-column or postcolumn mode; the latter offers interesting advantages, such as (i) it is in principle an automated flow-based step, (ii) the stability of the derivatives is not of concern, and (iii) it is more efficient when complicated matrixes are analyzed since each analyte is derivatized in "isolation" following the chromatographic separation. This way one of the critical disadvantages of the pre-column mode, that is potentially competition phenomena from the sample matrix, are avoided [26][27][28][29].…”
The first dispersive liquid liquid microextraction scheme followed by liquid chromatography-post column derivatization for the determination of the antiviral drug rimantadine in urine samples is demonstrated. The effect of the type and volume of organic extraction solvent, type and volume of disperser solvent, sample pH, ionic strength, extraction time, and centrifugation speed on the extraction efficiency were studied. Rimantadine and the internal standard (amantadine) were chromatographed using a reversed phase monolithic stationary phase with a mixture of equal volumes of methanol and phosphate buffer (pH = 3) as mobile phase. On-line postcolumn derivatization of the analyte was performed using a "two-stream" manifold with o-phthalaldehyde and N-acetyl-cysteine at alkaline medium. Under the optimized extraction conditions, the enrichment factor of rimantadine was 58. The linear range was 5-100 µg/L with correlation coefficient r of 0.9984 while the limit of detection achieved was 0.5 µg/L. The within-day and between-day precision for the tested concentration levels were less than 14.3% and the mean recoveries obtained from the spiked samples were ranged between 87.5 and 113.9%. The main advantages of the proposed method are the simplicity of operation, rapidity, low cost, and low limit of detection of the analyte. K E Y W O R D S rimantadine, dispersive liquid liquid microextraction, liquid chromatography, post-column derivatization, urine J Sep Sci 2020;43:631-638.2. The proposed DLLME scheme offers significant advantages including simplicity, low operation cost employing typical laboratory equipment, high extraction efficiency, and enrichment at a relative short extraction time.3. The sensitivity is almost 10-times higher compared to analogous methods using conventional SPE as sample treatment.4. Besides sensitivity, the combination of the DLLME with on-line PCD offers high selectivity, a feature that is always important in bioanalytical applications.
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