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Molecularly imprinted-solid phase extraction combined with simultaneous derivatization and dispersive liquid-liquid microextraction for selective extraction and preconcentration of methamphetamine and ecstasy from urine samples followed by gas chromatography.
J Chromatogr A. 2012 Jul 27; 1248:24-31.JC

Abstract

In this study, a developed technique was reported for extraction and pre-concentration of methamphetamine (MAMP) and 3,4-methylenedioxymethamphetamine (MDMA, ecstasy) from urine samples using molecularly imprinted-solid phase extraction (MISPE) along with simultaneous derivatization and dispersive liquid-liquid microextraction (DLLME). Molecularly imprinted microspheres as sorbent in solid phase extraction (SPE) procedure were synthesized using precipitation polymerization with MAMP as the template. Aqueous solution of the target analytes was passed through MAMP-MIP cartridge and the adsorbed analytes were then eluted with methanol. The collected eluate was mixed with butylchloroformate which served as the derivatization reagent as well as the extraction solvent. The mixture was immediately injected into deionized water. After centrifugation, 1 μL of the settled organic phase was injected into gas chromatography-flame ionization detection (GC-FID) or gas chromatography-mass spectrometry (GC-MS). Various experimental parameters affecting the performance of both of the steps (MISPE and DLLME) were thoroughly investigated. The calibration graphs were linear in the ranges of 10-1500 ng mL(-1) (MAMP) and 50-1500 ng mL(-1) (MDMA), and the detection limits (LODs) were 2 and 18 ng mL(-1), respectively. The relative standard deviations (%RSDs) obtained for six repeated experiments (100 ng mL(-1) of each drug) were 5.1% and 6.8% for MAMP and MDMA, respectively. The relative recoveries obtained for the analytes in human urine samples, spiked with different levels of each drug, were within the range of 80-88%.

Authors+Show Affiliations

Department of Analytical Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz, Iran. djozan@tabrizu.ac.irNo affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

Evaluation Study
Journal Article
Research Support, Non-U.S. Gov't

Language

eng

PubMed ID

22704883

Citation

Djozan, Djavanshir, et al. "Molecularly Imprinted-solid Phase Extraction Combined With Simultaneous Derivatization and Dispersive Liquid-liquid Microextraction for Selective Extraction and Preconcentration of Methamphetamine and Ecstasy From Urine Samples Followed By Gas Chromatography." Journal of Chromatography. A, vol. 1248, 2012, pp. 24-31.
Djozan D, Farajzadeh MA, Sorouraddin SM, et al. Molecularly imprinted-solid phase extraction combined with simultaneous derivatization and dispersive liquid-liquid microextraction for selective extraction and preconcentration of methamphetamine and ecstasy from urine samples followed by gas chromatography. J Chromatogr A. 2012;1248:24-31.
Djozan, D., Farajzadeh, M. A., Sorouraddin, S. M., & Baheri, T. (2012). Molecularly imprinted-solid phase extraction combined with simultaneous derivatization and dispersive liquid-liquid microextraction for selective extraction and preconcentration of methamphetamine and ecstasy from urine samples followed by gas chromatography. Journal of Chromatography. A, 1248, 24-31. https://doi.org/10.1016/j.chroma.2012.05.085
Djozan D, et al. Molecularly Imprinted-solid Phase Extraction Combined With Simultaneous Derivatization and Dispersive Liquid-liquid Microextraction for Selective Extraction and Preconcentration of Methamphetamine and Ecstasy From Urine Samples Followed By Gas Chromatography. J Chromatogr A. 2012 Jul 27;1248:24-31. PubMed PMID: 22704883.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Molecularly imprinted-solid phase extraction combined with simultaneous derivatization and dispersive liquid-liquid microextraction for selective extraction and preconcentration of methamphetamine and ecstasy from urine samples followed by gas chromatography. AU - Djozan,Djavanshir, AU - Farajzadeh,Mir Ali, AU - Sorouraddin,Saeed Mohammad, AU - Baheri,Tahmineh, Y1 - 2012/05/31/ PY - 2012/01/07/received PY - 2012/05/23/revised PY - 2012/05/24/accepted PY - 2012/6/19/entrez PY - 2012/6/19/pubmed PY - 2012/9/25/medline SP - 24 EP - 31 JF - Journal of chromatography. A JO - J Chromatogr A VL - 1248 N2 - In this study, a developed technique was reported for extraction and pre-concentration of methamphetamine (MAMP) and 3,4-methylenedioxymethamphetamine (MDMA, ecstasy) from urine samples using molecularly imprinted-solid phase extraction (MISPE) along with simultaneous derivatization and dispersive liquid-liquid microextraction (DLLME). Molecularly imprinted microspheres as sorbent in solid phase extraction (SPE) procedure were synthesized using precipitation polymerization with MAMP as the template. Aqueous solution of the target analytes was passed through MAMP-MIP cartridge and the adsorbed analytes were then eluted with methanol. The collected eluate was mixed with butylchloroformate which served as the derivatization reagent as well as the extraction solvent. The mixture was immediately injected into deionized water. After centrifugation, 1 μL of the settled organic phase was injected into gas chromatography-flame ionization detection (GC-FID) or gas chromatography-mass spectrometry (GC-MS). Various experimental parameters affecting the performance of both of the steps (MISPE and DLLME) were thoroughly investigated. The calibration graphs were linear in the ranges of 10-1500 ng mL(-1) (MAMP) and 50-1500 ng mL(-1) (MDMA), and the detection limits (LODs) were 2 and 18 ng mL(-1), respectively. The relative standard deviations (%RSDs) obtained for six repeated experiments (100 ng mL(-1) of each drug) were 5.1% and 6.8% for MAMP and MDMA, respectively. The relative recoveries obtained for the analytes in human urine samples, spiked with different levels of each drug, were within the range of 80-88%. SN - 1873-3778 UR - https://www.unboundmedicine.com/medline/citation/22704883/Molecularly_imprinted_solid_phase_extraction_combined_with_simultaneous_derivatization_and_dispersive_liquid_liquid_microextraction_for_selective_extraction_and_preconcentration_of_methamphetamine_and_ecstasy_from_urine_samples_followed_by_gas_chromatography_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S0021-9673(12)00817-5 DB - PRIME DP - Unbound Medicine ER -