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1.
J Pharm Biomed Anal ; 42(5): 549-55, 2006 Nov 16.
Artigo em Inglês | MEDLINE | ID: mdl-16859856

RESUMO

Non-covalent molecularly imprinted polymers (MIPs) of cholesterol were prepared by UV initiated polymerization. A polymer that had the highest binding selectivity and capability was used as solid-phase extraction (SPE) sorbents for direct extraction of cholesterol from different biological samples (human serum, cow milk, yolk, shrimp, pork and beef). The extraction conditions of molecularly imprinted SPE (MISPE) were optimized and the optimum protocol was: conditioning MISPE cartridges with n-hexane, loading with n-hexane, washing with n-hexane and n-hexane:toluene=9:1, respectively, then eluting with chloroform:ethanol:acetic acid=3:1:1. Cholesterol MISPE selectively recognized, effectively trapped and pre-concentrated cholesterol over a concentration range of 10-80 microg/mL. Recoveries ranged from 80.6% to 92.7%, with R.S.D. lower than 9.8%. Under the optimal condition, MISPE recoveries of spiked human serum, yolk, cow milk, shrimp, pork and beef were 91.1%, 80.4%, 86.6%, 78.2%, 81.4% and 80.1%, respectively. Compared with C18 SPE, almost all of the matrix interferences were removed after MISPE, and better baselines and higher selectivity were achieved.


Assuntos
Colesterol/análise , Análise de Alimentos/métodos , Polímeros/química , Extração em Fase Sólida/métodos , Animais , Bovinos , Colesterol/sangue , Gema de Ovo/química , Humanos , Carne/análise , Leite/química , Estrutura Molecular , Penaeidae/química , Sensibilidade e Especificidade , Suínos
2.
Anal Bioanal Chem ; 387(3): 1007-16, 2007 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-17186227

RESUMO

Molecularly imprinted polymers (MIPs) were prepared by precipitation polymerization using tebuconazole (TBZ) as a template. Frontal chromatography and selectivity experiments were used to determine the binding capabilities and binding specificities of different MIPs. The polymer that had the highest binding selectivity and capability was used as the solid-phase extraction (SPE) sorbent for the direct extraction of TBZ from different biological and environmental samples (cabbage, pannage, shrimp, orange juice and tap water). The extraction protocol was optimized and the optimum conditions were: conditioning with 5 mL methanol:acetic acid (9:1), 5 mL methanol and 5 mL water respectively, loading with 5 mL aqueous samples, washing with 1.2 mL acetonitrile (ACN):phosphate buffer (5:5, pH3), and eluting with 3 mL methanol. The MIPs were able to selectively recognize, effectively trap and preconcentrate TBZ over a concentration range of 0.5-15 micromol/L. The intraday and interday RSDs were less than 9.7% and 8.6%, respectively. The limit of quantification was 0.1 micromol/L. Under optimum conditions, the MISPE recoveries of spiked cabbage, pannage, shrimp, orange juice and tap water were 62.3%, 75.8%, 71.6%, 89% and 93.9%, respectively. MISPE gave better HPLC separation efficiencies and higher recoveries than C18 SPE and strong cation exchange (SCX) SPE.


Assuntos
Análise de Alimentos/métodos , Polímeros/química , Extração em Fase Sólida/métodos , Triazóis/química , Poluentes Químicos da Água/análise , Ácido Acético/química , Acetonitrilas/química , Soluções Tampão , Resinas de Troca de Cátion , Cromatografia Líquida de Alta Pressão/métodos , Metanol/química , Reprodutibilidade dos Testes , Sensibilidade e Especificidade , Fatores de Tempo
3.
Anal Bioanal Chem ; 385(4): 780-6, 2006 Jun.
Artigo em Inglês | MEDLINE | ID: mdl-16741779

RESUMO

Molecularly imprinted polymers (MIPs) were prepared using bisphenol A (BPA) as a template by precipitation polymerization. The polymer that had the highest binding selectivity and ability was used as solid-phase extraction (SPE) sorbents for direct extraction of BPA from different biological and environmental samples (human serum, pig urine, tap water and shrimp). The extraction protocol was optimized and the optimum conditions were as follows: conditioning with 5 mL methanol-acetic acid (3:1), 5 mL methanol, 5 mL acetonitrile and 5 mL water, respectively, loading with 5 mL aqueous samples, washing with 1 mL acetonitrile, and eluting with 3 mL methanol. MIPs can selectively recognize, effectively trap and preconcentrate BPA over a concentration range of 2-20 microM. Recoveries ranged from 94.03 to 105.3%, with a relative standard deviation lower than 7.9%. Under the optimal condition, molecularly imprinted SPE recoveries of spiked human serum, pig urine, tap water and shrimp were 65.80, 82.32, 76.00 and 75.97%, respectively, when aqueous samples were applied directly. Compared with C18 SPE, a better baseline, better high-performance liquid chromatography separation efficiency and higher recoveries were achieved after molecularly imprinted SPE.


Assuntos
Meio Ambiente , Fenóis/isolamento & purificação , Polímeros/química , Soro/química , Extração em Fase Sólida/métodos , Urina/química , Água/análise , Animais , Compostos Benzidrílicos , Cromatografia Líquida de Alta Pressão , Crustáceos , Humanos , Microscopia Eletrônica de Varredura , Estrutura Molecular , Fenóis/química , Reprodutibilidade dos Testes , Suínos
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