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Aqueous phase hexylchloroformate derivatization and solid phase microextraction: determination of benzoylecgonine in urine by gas chromatography-quadrupole ion trap mass spectrometry.
J Forensic Sci. 1999 May; 44(3):527-34.JF

Abstract

A derivatization/solid phase microextraction (SPME) method for the determination of benzoylecgonine in urine was developed. The derivatization is conducted directly in 1 mL of urine while sonicating for 3 min with 12 microL of hexyl chloroformate and 70 microL of a mixture containing acetonitrile:water:hexanol:2-dimethylaminopyridine (5:2:2:1 v/v), yielding benzoylecgonine hexyl ester (BHE) as the product. After the 3 min period, an aliquot of 250 microL is transferred to a vial for SPME. After the desired extraction time the 100 microns polydimethylsiloxane SPME fiber was transferred to the GC-MS for separation and analysis with a quadrupole ion trap mass spectrometer. The hexyl chloroformate derivatization and SPME procedures were optimized for compatibility and sensitivity. The method was found linear for 0.10 to 20.0 micrograms/mL (r2 = 0.999) of benzoylecgonine in urine using benzoylecgonine-d3 as an internal standard (1.5 micrograms/mL). Intra-day precisions were 8.8 and 6.8% RSD for 0.30 microgram/mL and 17 micrograms/mL benzoylecgonine standards in urine (n = 6), respectively. Inter-day precision (n = 3) were < or = 3.3% RSD, indicating good reproducibility. A detection limit of 0.03 microgram/mL (S/N = 3) was achieved, thus making the SPME method a simplified alternative to SPE for GC-MS confirmation after EMIT tests for benzoylecgonine which have a cutoff of 0.30 microgram/mL. Quantitative results by SPME and SPE of two clinical urine specimens known positive for cocaine by EMIT were in excellent agreement. Benzoylecgonine was detected by the derivatization/SPME method in 22 out of 22 other urine specimens known positive for cocaine.

Authors+Show Affiliations

Department of Chemistry and Biochemistry, University of Texas at Austin, USA.No affiliation info availableNo affiliation info available

Pub Type(s)

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

Language

eng

PubMed ID

10408106

Citation

Hall, B J., et al. "Aqueous Phase Hexylchloroformate Derivatization and Solid Phase Microextraction: Determination of Benzoylecgonine in Urine By Gas Chromatography-quadrupole Ion Trap Mass Spectrometry." Journal of Forensic Sciences, vol. 44, no. 3, 1999, pp. 527-34.
Hall BJ, Parikh AR, Brodbelt JS. Aqueous phase hexylchloroformate derivatization and solid phase microextraction: determination of benzoylecgonine in urine by gas chromatography-quadrupole ion trap mass spectrometry. J Forensic Sci. 1999;44(3):527-34.
Hall, B. J., Parikh, A. R., & Brodbelt, J. S. (1999). Aqueous phase hexylchloroformate derivatization and solid phase microextraction: determination of benzoylecgonine in urine by gas chromatography-quadrupole ion trap mass spectrometry. Journal of Forensic Sciences, 44(3), 527-34.
Hall BJ, Parikh AR, Brodbelt JS. Aqueous Phase Hexylchloroformate Derivatization and Solid Phase Microextraction: Determination of Benzoylecgonine in Urine By Gas Chromatography-quadrupole Ion Trap Mass Spectrometry. J Forensic Sci. 1999;44(3):527-34. PubMed PMID: 10408106.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Aqueous phase hexylchloroformate derivatization and solid phase microextraction: determination of benzoylecgonine in urine by gas chromatography-quadrupole ion trap mass spectrometry. AU - Hall,B J, AU - Parikh,A R, AU - Brodbelt,J S, PY - 1999/7/17/pubmed PY - 1999/7/17/medline PY - 1999/7/17/entrez SP - 527 EP - 34 JF - Journal of forensic sciences JO - J Forensic Sci VL - 44 IS - 3 N2 - A derivatization/solid phase microextraction (SPME) method for the determination of benzoylecgonine in urine was developed. The derivatization is conducted directly in 1 mL of urine while sonicating for 3 min with 12 microL of hexyl chloroformate and 70 microL of a mixture containing acetonitrile:water:hexanol:2-dimethylaminopyridine (5:2:2:1 v/v), yielding benzoylecgonine hexyl ester (BHE) as the product. After the 3 min period, an aliquot of 250 microL is transferred to a vial for SPME. After the desired extraction time the 100 microns polydimethylsiloxane SPME fiber was transferred to the GC-MS for separation and analysis with a quadrupole ion trap mass spectrometer. The hexyl chloroformate derivatization and SPME procedures were optimized for compatibility and sensitivity. The method was found linear for 0.10 to 20.0 micrograms/mL (r2 = 0.999) of benzoylecgonine in urine using benzoylecgonine-d3 as an internal standard (1.5 micrograms/mL). Intra-day precisions were 8.8 and 6.8% RSD for 0.30 microgram/mL and 17 micrograms/mL benzoylecgonine standards in urine (n = 6), respectively. Inter-day precision (n = 3) were < or = 3.3% RSD, indicating good reproducibility. A detection limit of 0.03 microgram/mL (S/N = 3) was achieved, thus making the SPME method a simplified alternative to SPE for GC-MS confirmation after EMIT tests for benzoylecgonine which have a cutoff of 0.30 microgram/mL. Quantitative results by SPME and SPE of two clinical urine specimens known positive for cocaine by EMIT were in excellent agreement. Benzoylecgonine was detected by the derivatization/SPME method in 22 out of 22 other urine specimens known positive for cocaine. SN - 0022-1198 UR - https://www.unboundmedicine.com/medline/citation/10408106/Aqueous_phase_hexylchloroformate_derivatization_and_solid_phase_microextraction:_determination_of_benzoylecgonine_in_urine_by_gas_chromatography_quadrupole_ion_trap_mass_spectrometry_ L2 - https://antibodies.cancer.gov/detail/CPTC-RRM2-2 DB - PRIME DP - Unbound Medicine ER -