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Simultaneous supercritical fluid extraction and chemical derivatization for the gas chromatographic-isotope dilution mass spectrometric determination of amphetamine and methamphetamine in urine.
J Chromatogr B Biomed Sci Appl. 2001 Aug 05; 759(1):17-26.JC

Abstract

An in-situ supercritical fluid extraction (SFE) and chemical derivatization (ChD) procedure followed by gas chromatography-isotope dilution mass spectrometry (GC-MS) for the determination of amphetamines in urine is described and evaluated. While using celite as the SFE wet-support, the one-pot sample pretreatment procedure also employs ammonium water to alkalize the urine matrix that contains protonated amphetamine (AP) and methamphetamine (MA). The mean recoveries achieved by simultaneous SFE-ChD, i.e., 95% (RSD=3.8%) for AP and 89% (RSD=4.0%) for MA, are significantly better than the corresponding overall recoveries obtained upon stepwise SFE-ChD, suggesting the unreacted trifluoroacetic anhydride (TFA) in the former procedure has strengthened the extracting power of CO, fluid as has been evidenced by a control test. As to GC-MS analysis, the optimal qualitative ions and quantitative ions of the respective analytes were determined via a rigorous evaluation process. Thus, the regression calibration curves for AP and MA in urine are linear within 100 approximately 50,000 ng/ml, with correlation coefficients typically exceeding 0.999. The limits of detection determined by two methods for AP and MA vary from 19 to 50 ng/ml, and limits of quantitation from 21 to 100 ng/ml. Precisions calculated for the triplicate analyses of AP and MA in a 500-ng/ml spiked control, two real-case samples and two quasi real-case samples, respectively, using regression calibration are typically below 10%. The method is simple and reliable. It may serve as an alternative to the existing confirmatory protocol for forensic urine drug testing.

Authors+Show Affiliations

Department of Forensic Science, Central Police University, Kueishan, Taoyuan, Taiwan.No affiliation info availableNo affiliation info available

Pub Type(s)

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

Language

eng

PubMed ID

11499622

Citation

Wang, S M., et al. "Simultaneous Supercritical Fluid Extraction and Chemical Derivatization for the Gas Chromatographic-isotope Dilution Mass Spectrometric Determination of Amphetamine and Methamphetamine in Urine." Journal of Chromatography. B, Biomedical Sciences and Applications, vol. 759, no. 1, 2001, pp. 17-26.
Wang SM, Giang YS, Ling YC. Simultaneous supercritical fluid extraction and chemical derivatization for the gas chromatographic-isotope dilution mass spectrometric determination of amphetamine and methamphetamine in urine. J Chromatogr B Biomed Sci Appl. 2001;759(1):17-26.
Wang, S. M., Giang, Y. S., & Ling, Y. C. (2001). Simultaneous supercritical fluid extraction and chemical derivatization for the gas chromatographic-isotope dilution mass spectrometric determination of amphetamine and methamphetamine in urine. Journal of Chromatography. B, Biomedical Sciences and Applications, 759(1), 17-26.
Wang SM, Giang YS, Ling YC. Simultaneous Supercritical Fluid Extraction and Chemical Derivatization for the Gas Chromatographic-isotope Dilution Mass Spectrometric Determination of Amphetamine and Methamphetamine in Urine. J Chromatogr B Biomed Sci Appl. 2001 Aug 5;759(1):17-26. PubMed PMID: 11499622.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Simultaneous supercritical fluid extraction and chemical derivatization for the gas chromatographic-isotope dilution mass spectrometric determination of amphetamine and methamphetamine in urine. AU - Wang,S M, AU - Giang,Y S, AU - Ling,Y C, PY - 2001/8/14/pubmed PY - 2002/1/5/medline PY - 2001/8/14/entrez SP - 17 EP - 26 JF - Journal of chromatography. B, Biomedical sciences and applications JO - J. Chromatogr. B Biomed. Sci. Appl. VL - 759 IS - 1 N2 - An in-situ supercritical fluid extraction (SFE) and chemical derivatization (ChD) procedure followed by gas chromatography-isotope dilution mass spectrometry (GC-MS) for the determination of amphetamines in urine is described and evaluated. While using celite as the SFE wet-support, the one-pot sample pretreatment procedure also employs ammonium water to alkalize the urine matrix that contains protonated amphetamine (AP) and methamphetamine (MA). The mean recoveries achieved by simultaneous SFE-ChD, i.e., 95% (RSD=3.8%) for AP and 89% (RSD=4.0%) for MA, are significantly better than the corresponding overall recoveries obtained upon stepwise SFE-ChD, suggesting the unreacted trifluoroacetic anhydride (TFA) in the former procedure has strengthened the extracting power of CO, fluid as has been evidenced by a control test. As to GC-MS analysis, the optimal qualitative ions and quantitative ions of the respective analytes were determined via a rigorous evaluation process. Thus, the regression calibration curves for AP and MA in urine are linear within 100 approximately 50,000 ng/ml, with correlation coefficients typically exceeding 0.999. The limits of detection determined by two methods for AP and MA vary from 19 to 50 ng/ml, and limits of quantitation from 21 to 100 ng/ml. Precisions calculated for the triplicate analyses of AP and MA in a 500-ng/ml spiked control, two real-case samples and two quasi real-case samples, respectively, using regression calibration are typically below 10%. The method is simple and reliable. It may serve as an alternative to the existing confirmatory protocol for forensic urine drug testing. SN - 1387-2273 UR - https://www.unboundmedicine.com/medline/citation/11499622/Simultaneous_supercritical_fluid_extraction_and_chemical_derivatization_for_the_gas_chromatographic_isotope_dilution_mass_spectrometric_determination_of_amphetamine_and_methamphetamine_in_urine_ L2 - https://medlineplus.gov/methamphetamine.html DB - PRIME DP - Unbound Medicine ER -