Abstract:This study presents a novel, sensitive and selective molecularly imprinted solid-phase extraction (MISPE)-spectrofluorimetric method for the removal and determination of atenolol from human urine. Molecularly imprinted and non-imprinted polymers were synthesized thermally using a radical chain polymerization technique and used as solid-phase extraction sorbents. Acrylic acid ethylene glycol dimethacrylate, dibenzoyl peroxide and dichloroethane were used as a functional monomer, cross-linker, initiator and poro… Show more
“…4. Previous development of ATE MI-SPE [8] only have recoveries 74.5–75.2% with IF value 4.18 this result is below our result and proved that our MI-SPE potential to be used as extraction tools of ATE from serum.Fig. 3Recoveries and imprinting factor value of blood serum spiked with ATE alone and mix of ATE with other β blockers.Fig.…”
Section: Resultsmentioning
confidence: 52%
“…Therefore, monitoring of ATE levels is required to detect drug abuse, particularly in athletes, as well as for proper dose regulation for patients. Several methods have been developed to analyze ATE in plasma and urine using molecular imprinted solid phase extraction (MI-SPE) as sample preparation before analysis [6, 7, 8]. Molecular imprinting polymer (MIP) is a technique that was developed to make a polymer with specific molecular recognition to the specified compound [9, 10, 11, 12, 13].…”
Section: Introductionmentioning
confidence: 99%
“…The resulting sorbent has a more homogeneous physical size, so no grinding is required and the resulting polymer generally has a better adsorption profile than the bulk polymerization method [22]. All development of MI-SPE ATE that other researcher already done [6, 7, 8], none of them using precipitation polymerization and the result of recoveries are below 80%.…”
Atenolol (ATE) is a cardio-selective β-blocker that is used in the treatment of hypertension over extended periods. However, ATE, like propranolol, has major potential for misuse as a performance-enhancing drug in several sports. Therefore, an efficient and selective separation method is required to detect and monitor the level of ATE in the body. This paper presents a molecularly imprinted polymer with specific and selective binding to ATE using precipitation polymerization. We show that when employed in an optimized molecular imprinted solid phase extraction (MI-SPE) protocol, recoveries of 93.65 ± 1.29% from spiked blood serum with excellent discrimination from other β-blocker drugs is possible. The methodology used in this study includes molecular modeling interaction between ATE and itaconic acid (ITA) as functional monomer, followed by determination of binding constants with spectrophotometry, synthesis of the polymer using precipitation polymerization and ending with characterization and application of polymers to extract ATE in serum. Docking analysis revealed a binding affinity between ATE and ITA of −2.0 kcal/mol with the formation of hydrogen bonding. The association constant between ATE and ITA was studied by UV titration in two different solvents, with evidence of an association constant 6.277 × 10
2
M
−1
measured in acetonitrile: methanol (1:1). An optimized MI-SPE protocol was developed for the extraction of ATE from spiked blood serum, obtaining recoveries of 93.65% with excellent selectivity toward other β-blocker drugs.
“…4. Previous development of ATE MI-SPE [8] only have recoveries 74.5–75.2% with IF value 4.18 this result is below our result and proved that our MI-SPE potential to be used as extraction tools of ATE from serum.Fig. 3Recoveries and imprinting factor value of blood serum spiked with ATE alone and mix of ATE with other β blockers.Fig.…”
Section: Resultsmentioning
confidence: 52%
“…Therefore, monitoring of ATE levels is required to detect drug abuse, particularly in athletes, as well as for proper dose regulation for patients. Several methods have been developed to analyze ATE in plasma and urine using molecular imprinted solid phase extraction (MI-SPE) as sample preparation before analysis [6, 7, 8]. Molecular imprinting polymer (MIP) is a technique that was developed to make a polymer with specific molecular recognition to the specified compound [9, 10, 11, 12, 13].…”
Section: Introductionmentioning
confidence: 99%
“…The resulting sorbent has a more homogeneous physical size, so no grinding is required and the resulting polymer generally has a better adsorption profile than the bulk polymerization method [22]. All development of MI-SPE ATE that other researcher already done [6, 7, 8], none of them using precipitation polymerization and the result of recoveries are below 80%.…”
Atenolol (ATE) is a cardio-selective β-blocker that is used in the treatment of hypertension over extended periods. However, ATE, like propranolol, has major potential for misuse as a performance-enhancing drug in several sports. Therefore, an efficient and selective separation method is required to detect and monitor the level of ATE in the body. This paper presents a molecularly imprinted polymer with specific and selective binding to ATE using precipitation polymerization. We show that when employed in an optimized molecular imprinted solid phase extraction (MI-SPE) protocol, recoveries of 93.65 ± 1.29% from spiked blood serum with excellent discrimination from other β-blocker drugs is possible. The methodology used in this study includes molecular modeling interaction between ATE and itaconic acid (ITA) as functional monomer, followed by determination of binding constants with spectrophotometry, synthesis of the polymer using precipitation polymerization and ending with characterization and application of polymers to extract ATE in serum. Docking analysis revealed a binding affinity between ATE and ITA of −2.0 kcal/mol with the formation of hydrogen bonding. The association constant between ATE and ITA was studied by UV titration in two different solvents, with evidence of an association constant 6.277 × 10
2
M
−1
measured in acetonitrile: methanol (1:1). An optimized MI-SPE protocol was developed for the extraction of ATE from spiked blood serum, obtaining recoveries of 93.65% with excellent selectivity toward other β-blocker drugs.
“…Atenolol levels in the blood are very low, at 600 ng/mL three hours after the first dose and 50-70 ng/mL after 24 hours [6]. One SPE technique that is selective and able to eliminate the interfering matrix and concentrate analytes for detection is molecularly imprinted polymer (MIP) technology [7][8][9].…”
A monolithic imprinted atenolol column was constructed by in situ polymerisation using a methacrylic acid monomer and a 1 : 1 (v/v) porogen of propanol: toluene with two template: monomer: crosslinker combinations, namely, MIP 1 (1 : 4 : 20) and MIP 2 (1 : 5 : 20). Physical characterisation of the monolithic columns consisted of permeability testing, Fourier transform infrared (FTIR) testing, surface area analysis (SAA), and scanning electron microscopy (SEM). The permeability value of four monolithic columns was in the good category: MIP 1 (24.01 mD), NIP 1 (56.43 mD), MIP 2 (23.03 mD), and NIP 2 (14.47 mD). The polymerisation process of these four monolithic imprinted columns was carried out perfectly, as shown by the absence of vinyl groups (1000 cm−1 and 900 cm−1) during FTIR testing. Based on SAA testing, the pores of the four polymers were classified as mesopores. The best monolithic column was MIP 1, as seen from the intercolumn and intracolumn reproducibility values and a % RSD <2.0%. The MIP 1 column was selective towards atenolol, as seen from the selectivity factor, imprinting factor (IF), and resolution (Rs) values. The IF values of MIP 1 were atenolol (204.62), metoprolol (3.36), and propranolol (1.27). The Rs value between atenolol and the analogue compounds was 7.23. The MIP 1 column can be used for the analysis of atenolol in blood serum samples with an average percentage recovery rate of 94.88 ± 4.43%.
“…Methyl methacrylate is a functional monomer that can act as a hydrogen bond acceptor to its template [4]. Other researchers have done research on MI-SPE for atenolol [5–7], but none of them used precipitation polymerization as we used in this study, and the recoveries are below 80%. The porogen chosen in this study is propanol because it has low polarity that can reduce interference during the polymerization process and increase the number of MIP-binding sites [8].…”
Atenolol is one of the beta-1 blocker drugs that is misused by athletes to increase their performance during competition. Therefore, it is important to analyze atenolol levels in blood selectively. The preparation method that can be used in separating atenolol in sample is molecular imprinting solid-phase extraction (MI-SPE) because it has good selectivity and sensitivity. This study aims to examine the characteristics and analytical performance of imprinted polymers synthesized from functional monomer methyl methacrylate. The stages of this study include the determination of association constants, synthesis of sorbent MI-SPE atenolol using the bulk polymerization method, and precipitation with atenolol as the template, methyl methacrylate as the functional monomer, and propanol as the porogen. The template was extracted from a polymer, and then, the adsorption ability, capacity, and selectivity of MI-SPE and finally the application of the best MI-SPE to spiked serum samples were determined. MI-SPE was also characterized by using Fourier-transform instrument infrared (FTIR) and scanning electron microscope (SEM). The result of characterization with FTIR and SEM showed that MIP made by the precipitation polymerization method was completely polymerized, more porous, and produced smaller particle size with an average value of 0.274 μm. It had better analytic performances than MIP made by bulk polymerization, with affinity value 0.3607 mg/g and homogeneity value 1.3246, and good selectivity toward atenolol with imprinting factor value 22.519. Application of MI-SPE to spiked serum samples has an excellent recovery percentage of 95.46% over 0% for the nonimprinting one. Based on the result of study, MIP made by precipitation polymerization could be used to extract atenolol on serum samples toward drug analysis.
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