scholarly journals Synthesis and Evaluation of Molecularly Imprinted Polymer for the Determination of the Phthalate Esters in the Bottled Beverages by HPLC

2013 ◽  
Vol 2013 ◽  
pp. 1-9 ◽  
Author(s):  
Ya-Feng Jin ◽  
Yi-Jun Zhang ◽  
Yu-Ping Zhang ◽  
Jun Chen ◽  
Xiao-Mao Zhou ◽  
...  

A molecularly imprinted polymer (MIP) was prepared in acetonitrile by bulk polymerization, using di-n-octylphthalate (DOP) as a template molecular,α-methacrylic acid (MAA) as a functional monomer, and ethylene dimethacrylate (EDMA) as a crosslinker. Characterization and evaluation of the prepared MIP were carried out by scanning electron microscope (SEM), infrared absorption spectroscopy (IR), and the Scatchard analysis, respectively. Through the optimization of washing solvent, eluting solvent amount, flow rate of loading solution, and loading sample volume, an analysis method was established for DOP related compounds with high selectivity and sensitivity by using the selective molecularly imprinted solid-phase extraction (MI-SPE) technique. Moreover, under the optimal conditions, the extraction effects were comparatively investigated by using MIP cartridge, NIP cartridge, and the commercial PLS cartridge used especially for phthalic acid esters (PAEs), respectively. The results showed that the recoveries of spiked PAEs are in the range of 90.4%–97.8% with the relative standard deviation (RSD) of 1.6%–3.8% on the resulted MIP cartridge, whilst lower recoveries were obtained ranging from 80.2% to 88.9% with an RSD of 1.4%–5.2% on the commercial PLS cartridge.

Author(s):  
Meilia Suherman ◽  
Ike Susanti ◽  
Driyanti Rahayu ◽  
Rimadani Pratiwi ◽  
Aliya Nur Hasanah

Atenolol is a cardiovascular drug that has a narrow therapeutic index with long-term use and it’s often used as doping. Atenolol has a small concentration in human boby and it’s in  biological matrix (serum) so in the testing need a selective extraction so  the analyte can be pra-concentration and removed from matrix. Two molecularly imprinted polymers (MIPs) on propanol as porogen  have been made with two different methods i.e. bulk polymerization and precipitation polymerization. The polymer was made using atenolol as a template, methacrylic acid as a functional monomer, and ethylene glycol dimethacrylate as a crosslinker. Prformance evaluations showed that polymers from bulk polymerization provide better performance than polymers from precipitation polymerization when tested against standard solution. However, this sorbent has low  recovery percentage after applied into serum sample and could not be used as alternative for atenolol extraction in human serum.Key words: Molecularly imprinted polymer, Atenolol, Solid Phase Extraction, Preparation  method, propanol.


2011 ◽  
Vol 4 (4) ◽  
pp. 375-383 ◽  
Author(s):  
D. De Smet ◽  
P. Dubruel ◽  
C. Van Peteghem ◽  
S. De Saeger

The design of imprinted polymers selective towards patulin (PAT) and their application in food analysis are reported for the first time. Different templates, functional monomers and molar ratios were evaluated related to binding capacity and specificity. Besides the toxin itself, the implementation of structural analogues (2-hydroxynicotinic acid, 5-indanol and 3-hydroxyphtalic anhydride) as templates was evaluated. A molecularly imprinted solid-phase extraction (MISPE) procedure was optimised for the selective clean-up of apple juice samples. Depending on the spiked concentration, recoveries after MISPE and non-imprinted solid-phase extraction varied respectively from 60% to 66% and from 40% to 41%. Limit of detection and limit of quantification were 10.0 µg/kg and 33.3 µg/kg, respectively. Equilibrium experiments and Scatchard analysis disclosed the presence of two classes of binding sites in the imprinted polymer. The dissociation constant (KD) of the higher affinity binding sites was 3.3 µmol/l, while the KD of the lower affinity binding sites was 260.7 µmol/l. The performance of the molecularly imprinted polymer throughout the clean-up was compared to liquid-liquid extraction and a C18 sorbent. Cross-reactivity experiments demonstrated that MISPE was substantially more selective than C18 clean-up. Moreover chromatograms, with less interfering peaks, were observed with MISPE resulting in a sensitive and reliable quantification of PAT.


2019 ◽  
Vol 79 (2) ◽  
pp. 356-365 ◽  
Author(s):  
Sinothando P. Mtolo ◽  
Precious N. Mahlambi ◽  
Lawrence M. Madikizela

Abstract Efavirenz is one of the antiretroviral drugs widely used to treat the human immunodeficiency virus. Antiretroviral drugs have been found to be present in surface water and wastewater. Due to complexity of environmental samples, solid-phase extraction (SPE) is used for isolation and pre-concentration of antiretroviral drugs prior to their chromatographic analysis. However, the commercially available SPE sorbents lack selectivity, which tends to prolong the analysis time. Therefore, in this study a molecularly imprinted polymer was synthesized for the specific recognition of efavirenz and then applied as the SPE sorbent for its extraction from wastewater and surface water samples. The imprinted and non-imprinted polymers were synthesized using a bulk polymerization technique where efavirenz was used as the template, 2-vinylpyridine as functional monomer, 1,1′-azobis-(cyclohexanecarbonitrile) as initiator, ethylene glycol dimethacrylate as cross-linker and toluene:acetonitrile (9:1, v/v) as the porogenic solvent mixture. The characterization was performed using Fourier transform infrared spectroscopy, scanning electron microscopy, Brunauer–Emmett–Teller, elemental analysis, and thermogravimetric analysis techniques. Results showed better selectivity of molecularly imprinted polymer to efavirenz than did non-imprinted polymer. The analysis was performed using high performance liquid chromatography equipped with a photo-diode array detector. The analytical method gave a detection limit of 0.41 μg/L and the analyte recovery of 81% in wastewater. The concentrations found in wastewater ranged from 2.79 to 120.7 μg/L, while in surface water they were between 0.975 and 2.88 μg/L. Therefore, the results of this study show a strong need for a detailed screening of efavirenz in major water utilities in the country.


2021 ◽  
Vol 11 (5) ◽  
pp. 13524-13534

Methoxyfenozide-selective surface molecularly imprinted polymer (MIP) sorbent was synthesized by reversible addition-fragmentation chain transfer (RAFT) polymerization based on support matrix of SBA-15. The size, morphology, composition, and properties of the prepared nanocomposite have also been characterized and determined using scanning electron microscopy (SEM) and Fourier-transform- infrared (FT-IR) spectroscopy. A miniaturized solid-phase extraction procedure has been developed for ultra-trace determination of methoxyfenozide adsorbed on polymethacrylic acid-functionalized Santa Barbara Amorphous type material (SBA-15), which is packed into a pipette- tip (PT). The PT-SPE was assembled by packing 2.0 mg of nanocomposite of MIP as sorbent into a 100 μL pipette tip. The method was optimized for several important extraction parameters such as sample volume, pH, amount of sorbent, and eluent solvent. The results determine that the prepared adsorbent has a high extraction power. High sensitivity, non-use of organic solvent, high selectivity, and low detection limits are the unique advantages of the proposed method.


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