Synthesis by precipitation polymerisation of molecularly imprinted polymer microspheres for the selective extraction of carbamazepine and oxcarbazepine from human urine

A. Beltran, R.M. Marce, P.A.G. Cormack, F. Borrull

Research output: Contribution to journalArticle

93 Citations (Scopus)

Abstract

Two molecularly imprinted polymers (MIPs), in the physical form of well-defined polymer microspheres, were synthesised via precipitation polymerisation (PP) using an antiepileptic drug, carbamazepine (CBZ), as template molecule, methacrylic acid as functional monomer and either divinylbenzene 80 (DVB-80) or a mixture of DVB-80 and ethylene glycol dimethacrylate (EGDMA) as crosslinking agents. The MIP obtained using DVB-80 alone as crosslinking agent (MIP A) had a narrow particle size distribution (9.5 +/- 0.5 mu m) and a well-developed permanent pore structure (specific surface area in the dry state = 758 m(2) g(-1)), whereas when a mixture of DVB-80 and EGDMA (MIP B) were used as crosslinking agents, the polymer obtained had a broader particle size distribution (6.4 +/- 1.8 mu m) and a relatively low specific surface area (23 m(2) g(-1)). The molecular recognition character of both polymers was evaluated by means of LC and then a molecularly imprinted solid-phase extraction (MISPE) protocol; CBZ was recognised by both polymers, and useful cross-selectivity for oxcarbazepine (OCBZ), which is the main metabolite of CBZ, also observed. In a detailed bioanalytical study, MIP A was selected in preference to MIP B since MIP A enabled a high volume of sample to be extracted such that lower limits of detection were achievable using this polymer. High recoveries of CBZ and OCBZ were obtained in a MISPE protocol when 50 mL of human urine spiked at 0.2 mg L-1 were percolated through MIP A (90% and 83%, respectively).
LanguageEnglish
Pages2248-2253
Number of pages6
JournalJournal of Chromatography A
Volume1216
Issue number12
DOIs
Publication statusPublished - 20 Mar 2009

Fingerprint

Carbamazepine
Microspheres
Polymerization
Polymers
divinyl benzene
Urine
Crosslinking
Solid Phase Extraction
Particle Size
Specific surface area
Particle size analysis
oxcarbazepine
Molecular recognition
Pore structure
Metabolites
Anticonvulsants
Limit of Detection
Monomers

Keywords

  • molecularly imprinted polymer
  • carbamazepine
  • oxcarbazepine
  • solid-phase extraction
  • precipitation polymerisation

Cite this

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title = "Synthesis by precipitation polymerisation of molecularly imprinted polymer microspheres for the selective extraction of carbamazepine and oxcarbazepine from human urine",
abstract = "Two molecularly imprinted polymers (MIPs), in the physical form of well-defined polymer microspheres, were synthesised via precipitation polymerisation (PP) using an antiepileptic drug, carbamazepine (CBZ), as template molecule, methacrylic acid as functional monomer and either divinylbenzene 80 (DVB-80) or a mixture of DVB-80 and ethylene glycol dimethacrylate (EGDMA) as crosslinking agents. The MIP obtained using DVB-80 alone as crosslinking agent (MIP A) had a narrow particle size distribution (9.5 +/- 0.5 mu m) and a well-developed permanent pore structure (specific surface area in the dry state = 758 m(2) g(-1)), whereas when a mixture of DVB-80 and EGDMA (MIP B) were used as crosslinking agents, the polymer obtained had a broader particle size distribution (6.4 +/- 1.8 mu m) and a relatively low specific surface area (23 m(2) g(-1)). The molecular recognition character of both polymers was evaluated by means of LC and then a molecularly imprinted solid-phase extraction (MISPE) protocol; CBZ was recognised by both polymers, and useful cross-selectivity for oxcarbazepine (OCBZ), which is the main metabolite of CBZ, also observed. In a detailed bioanalytical study, MIP A was selected in preference to MIP B since MIP A enabled a high volume of sample to be extracted such that lower limits of detection were achievable using this polymer. High recoveries of CBZ and OCBZ were obtained in a MISPE protocol when 50 mL of human urine spiked at 0.2 mg L-1 were percolated through MIP A (90{\%} and 83{\%}, respectively).",
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Synthesis by precipitation polymerisation of molecularly imprinted polymer microspheres for the selective extraction of carbamazepine and oxcarbazepine from human urine. / Beltran, A.; Marce, R.M.; Cormack, P.A.G.; Borrull, F.

In: Journal of Chromatography A , Vol. 1216, No. 12, 20.03.2009, p. 2248-2253.

Research output: Contribution to journalArticle

TY - JOUR

T1 - Synthesis by precipitation polymerisation of molecularly imprinted polymer microspheres for the selective extraction of carbamazepine and oxcarbazepine from human urine

AU - Beltran, A.

AU - Marce, R.M.

AU - Cormack, P.A.G.

AU - Borrull, F.

PY - 2009/3/20

Y1 - 2009/3/20

N2 - Two molecularly imprinted polymers (MIPs), in the physical form of well-defined polymer microspheres, were synthesised via precipitation polymerisation (PP) using an antiepileptic drug, carbamazepine (CBZ), as template molecule, methacrylic acid as functional monomer and either divinylbenzene 80 (DVB-80) or a mixture of DVB-80 and ethylene glycol dimethacrylate (EGDMA) as crosslinking agents. The MIP obtained using DVB-80 alone as crosslinking agent (MIP A) had a narrow particle size distribution (9.5 +/- 0.5 mu m) and a well-developed permanent pore structure (specific surface area in the dry state = 758 m(2) g(-1)), whereas when a mixture of DVB-80 and EGDMA (MIP B) were used as crosslinking agents, the polymer obtained had a broader particle size distribution (6.4 +/- 1.8 mu m) and a relatively low specific surface area (23 m(2) g(-1)). The molecular recognition character of both polymers was evaluated by means of LC and then a molecularly imprinted solid-phase extraction (MISPE) protocol; CBZ was recognised by both polymers, and useful cross-selectivity for oxcarbazepine (OCBZ), which is the main metabolite of CBZ, also observed. In a detailed bioanalytical study, MIP A was selected in preference to MIP B since MIP A enabled a high volume of sample to be extracted such that lower limits of detection were achievable using this polymer. High recoveries of CBZ and OCBZ were obtained in a MISPE protocol when 50 mL of human urine spiked at 0.2 mg L-1 were percolated through MIP A (90% and 83%, respectively).

AB - Two molecularly imprinted polymers (MIPs), in the physical form of well-defined polymer microspheres, were synthesised via precipitation polymerisation (PP) using an antiepileptic drug, carbamazepine (CBZ), as template molecule, methacrylic acid as functional monomer and either divinylbenzene 80 (DVB-80) or a mixture of DVB-80 and ethylene glycol dimethacrylate (EGDMA) as crosslinking agents. The MIP obtained using DVB-80 alone as crosslinking agent (MIP A) had a narrow particle size distribution (9.5 +/- 0.5 mu m) and a well-developed permanent pore structure (specific surface area in the dry state = 758 m(2) g(-1)), whereas when a mixture of DVB-80 and EGDMA (MIP B) were used as crosslinking agents, the polymer obtained had a broader particle size distribution (6.4 +/- 1.8 mu m) and a relatively low specific surface area (23 m(2) g(-1)). The molecular recognition character of both polymers was evaluated by means of LC and then a molecularly imprinted solid-phase extraction (MISPE) protocol; CBZ was recognised by both polymers, and useful cross-selectivity for oxcarbazepine (OCBZ), which is the main metabolite of CBZ, also observed. In a detailed bioanalytical study, MIP A was selected in preference to MIP B since MIP A enabled a high volume of sample to be extracted such that lower limits of detection were achievable using this polymer. High recoveries of CBZ and OCBZ were obtained in a MISPE protocol when 50 mL of human urine spiked at 0.2 mg L-1 were percolated through MIP A (90% and 83%, respectively).

KW - molecularly imprinted polymer

KW - carbamazepine

KW - oxcarbazepine

KW - solid-phase extraction

KW - precipitation polymerisation

U2 - 10.1016/j.chroma.2009.01.024

DO - 10.1016/j.chroma.2009.01.024

M3 - Article

VL - 1216

SP - 2248

EP - 2253

JO - Journal of Chromatography A

T2 - Journal of Chromatography A

JF - Journal of Chromatography A

SN - 0021-9673

IS - 12

ER -