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Monolithic silica spin column extraction and simultaneous derivatization of amphetamines and 3,4-methylenedioxyamphetamines in human urine for gas chromatographic-mass spectrometric detection.
Anal Chim Acta. 2010 Feb 19; 661(1):42-6.AC

Abstract

A simple, sensitive, and specific method with gas chromatography-mass spectrometry was developed for simultaneous extraction and derivatization of amphetamines (APs) and 3,4-methylenedioxyamphetamines (MDAs) in human urine by using a monolithic silica spin column. All the procedures, such as sample loading, washing, and elution were performed by centrifugation. APs and MDAs in urine were adsorbed on the monolithic silica and derivatized with propyl chloroformate in the column. Methamphetamine-d(5) was used as an internal standard. The linear ranges were 0.01-5.0 microg mL(-1) for methamphetamine (MA) and 3,4-methylenedioxymethamphetamine (MDMA) and 0.02-5.0 microg mL(-1) for amphetamine (AP) and 3,4-methylenedioxyamphetamine (MDA) (coefficient of correlation > or = 0.995). The recovery of APs and MDAs in urine was 84-94%, and the relative standard deviation of the intra- and interday reproducibility for urine samples containing 0.1, 1.0, and 4.0 microg mL(-1) of APs and MDAs ranged from 1.4% to 13.6%. The lowest detection limit (signal-to-noise ratio > or = 3) in urine was 5 ng mL(-1) for MA and MDMA and 10 ng mL(-1) for AP and MDA. The proposed method can be used to perform simultaneous extraction and derivatization on spin columns that have been loaded with a small quantity of solvent by using centrifugation.

Authors+Show Affiliations

Scientific Investigation Laboratory, Hiroshima Prefectural Police Headquarters, Kohnan 2-26-3, Naka-ku, Hiroshima 730-0825, Japan.No affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

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

Language

eng

PubMed ID

20113714

Citation

Nakamoto, Akihiro, et al. "Monolithic Silica Spin Column Extraction and Simultaneous Derivatization of Amphetamines and 3,4-methylenedioxyamphetamines in Human Urine for Gas Chromatographic-mass Spectrometric Detection." Analytica Chimica Acta, vol. 661, no. 1, 2010, pp. 42-6.
Nakamoto A, Nishida M, Saito T, et al. Monolithic silica spin column extraction and simultaneous derivatization of amphetamines and 3,4-methylenedioxyamphetamines in human urine for gas chromatographic-mass spectrometric detection. Anal Chim Acta. 2010;661(1):42-6.
Nakamoto, A., Nishida, M., Saito, T., Kishiyama, I., Miyazaki, S., Murakami, K., Nagao, M., & Namura, A. (2010). Monolithic silica spin column extraction and simultaneous derivatization of amphetamines and 3,4-methylenedioxyamphetamines in human urine for gas chromatographic-mass spectrometric detection. Analytica Chimica Acta, 661(1), 42-6. https://doi.org/10.1016/j.aca.2009.12.013
Nakamoto A, et al. Monolithic Silica Spin Column Extraction and Simultaneous Derivatization of Amphetamines and 3,4-methylenedioxyamphetamines in Human Urine for Gas Chromatographic-mass Spectrometric Detection. Anal Chim Acta. 2010 Feb 19;661(1):42-6. PubMed PMID: 20113714.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Monolithic silica spin column extraction and simultaneous derivatization of amphetamines and 3,4-methylenedioxyamphetamines in human urine for gas chromatographic-mass spectrometric detection. AU - Nakamoto,Akihiro, AU - Nishida,Manami, AU - Saito,Takeshi, AU - Kishiyama,Izumi, AU - Miyazaki,Shota, AU - Murakami,Katsunori, AU - Nagao,Masataka, AU - Namura,Akira, Y1 - 2009/12/16/ PY - 2009/06/22/received PY - 2009/12/11/revised PY - 2009/12/11/accepted PY - 2010/2/2/entrez PY - 2010/2/2/pubmed PY - 2010/4/1/medline SP - 42 EP - 6 JF - Analytica chimica acta JO - Anal. Chim. Acta VL - 661 IS - 1 N2 - A simple, sensitive, and specific method with gas chromatography-mass spectrometry was developed for simultaneous extraction and derivatization of amphetamines (APs) and 3,4-methylenedioxyamphetamines (MDAs) in human urine by using a monolithic silica spin column. All the procedures, such as sample loading, washing, and elution were performed by centrifugation. APs and MDAs in urine were adsorbed on the monolithic silica and derivatized with propyl chloroformate in the column. Methamphetamine-d(5) was used as an internal standard. The linear ranges were 0.01-5.0 microg mL(-1) for methamphetamine (MA) and 3,4-methylenedioxymethamphetamine (MDMA) and 0.02-5.0 microg mL(-1) for amphetamine (AP) and 3,4-methylenedioxyamphetamine (MDA) (coefficient of correlation > or = 0.995). The recovery of APs and MDAs in urine was 84-94%, and the relative standard deviation of the intra- and interday reproducibility for urine samples containing 0.1, 1.0, and 4.0 microg mL(-1) of APs and MDAs ranged from 1.4% to 13.6%. The lowest detection limit (signal-to-noise ratio > or = 3) in urine was 5 ng mL(-1) for MA and MDMA and 10 ng mL(-1) for AP and MDA. The proposed method can be used to perform simultaneous extraction and derivatization on spin columns that have been loaded with a small quantity of solvent by using centrifugation. SN - 1873-4324 UR - https://www.unboundmedicine.com/medline/citation/20113714/Monolithic_silica_spin_column_extraction_and_simultaneous_derivatization_of_amphetamines_and_34_methylenedioxyamphetamines_in_human_urine_for_gas_chromatographic_mass_spectrometric_detection_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S0003-2670(09)01666-3 DB - PRIME DP - Unbound Medicine ER -