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Automated determination of 'Ecstasy' and amphetamines in urine by SPME and capillary gas chromatography after propylchloroformate derivatisation.
J Pharm Biomed Anal. 1999 Mar; 19(3-4):463-75.JP

Abstract

The determination of amphetamines and their methylenedioxylated analogs in urine by propylchloroformate derivatisation and automated solid-phase microextraction is described. The urine sample was adjusted to pH 10.8 and added propylchloroformate reagent and an internal standard. Derivatisation resulted in water-stable carbamates which were automatically extracted by solid-phase microextraction. A fiber coated with polydimethylsiloxane was inserted into the urine matrix and agitated for 16 min. The fibre with the extracted carbamates was injected into the heated split-splitless injection port of the gas chromatograph where the analytes were evaporated at 300 degrees C, separated on a methylsilicone capillary column and detected by either a nitrogen phosphorous detector or by mass spectrometry. The method was shown to be highly reproducible and robust with respect to variations in the urine matrices. The detection limits were 5 ng/ml(-1) of methamphetamine, MDMA and MDEA and 15 ng/ml(-1) of amphetamine and MDA in urine. The method is a solvent free, automated alternative to traditional methods for determination of the amphetamine and their methylendioxylated analogs in urine.

Authors+Show Affiliations

Institute of Pharmacy, University of Oslo, Norway.No affiliation info availableNo affiliation info available

Pub Type(s)

Journal Article

Language

eng

PubMed ID

10704112

Citation

Ugland, H G., et al. "Automated Determination of 'Ecstasy' and Amphetamines in Urine By SPME and Capillary Gas Chromatography After Propylchloroformate Derivatisation." Journal of Pharmaceutical and Biomedical Analysis, vol. 19, no. 3-4, 1999, pp. 463-75.
Ugland HG, Krogh M, Rasmussen KE. Automated determination of 'Ecstasy' and amphetamines in urine by SPME and capillary gas chromatography after propylchloroformate derivatisation. J Pharm Biomed Anal. 1999;19(3-4):463-75.
Ugland, H. G., Krogh, M., & Rasmussen, K. E. (1999). Automated determination of 'Ecstasy' and amphetamines in urine by SPME and capillary gas chromatography after propylchloroformate derivatisation. Journal of Pharmaceutical and Biomedical Analysis, 19(3-4), 463-75.
Ugland HG, Krogh M, Rasmussen KE. Automated Determination of 'Ecstasy' and Amphetamines in Urine By SPME and Capillary Gas Chromatography After Propylchloroformate Derivatisation. J Pharm Biomed Anal. 1999;19(3-4):463-75. PubMed PMID: 10704112.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Automated determination of 'Ecstasy' and amphetamines in urine by SPME and capillary gas chromatography after propylchloroformate derivatisation. AU - Ugland,H G, AU - Krogh,M, AU - Rasmussen,K E, PY - 2000/3/7/pubmed PY - 2000/3/25/medline PY - 2000/3/7/entrez SP - 463 EP - 75 JF - Journal of pharmaceutical and biomedical analysis JO - J Pharm Biomed Anal VL - 19 IS - 3-4 N2 - The determination of amphetamines and their methylenedioxylated analogs in urine by propylchloroformate derivatisation and automated solid-phase microextraction is described. The urine sample was adjusted to pH 10.8 and added propylchloroformate reagent and an internal standard. Derivatisation resulted in water-stable carbamates which were automatically extracted by solid-phase microextraction. A fiber coated with polydimethylsiloxane was inserted into the urine matrix and agitated for 16 min. The fibre with the extracted carbamates was injected into the heated split-splitless injection port of the gas chromatograph where the analytes were evaporated at 300 degrees C, separated on a methylsilicone capillary column and detected by either a nitrogen phosphorous detector or by mass spectrometry. The method was shown to be highly reproducible and robust with respect to variations in the urine matrices. The detection limits were 5 ng/ml(-1) of methamphetamine, MDMA and MDEA and 15 ng/ml(-1) of amphetamine and MDA in urine. The method is a solvent free, automated alternative to traditional methods for determination of the amphetamine and their methylendioxylated analogs in urine. SN - 0731-7085 UR - https://www.unboundmedicine.com/medline/citation/10704112/Automated_determination_of_'Ecstasy'_and_amphetamines_in_urine_by_SPME_and_capillary_gas_chromatography_after_propylchloroformate_derivatisation_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S0731-7085(98)00240-4 DB - PRIME DP - Unbound Medicine ER -