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Quantitation of methamphetamine and amphetamine in urine by capillary GC/MS Part II. Derivatization with 4-carbethoxyhexafluorobutyryl chloride.
J Anal Toxicol. 1989 Sep-Oct; 13(5):257-62.JA

Abstract

An analytical procedure for methamphetamine and amphetamine has been developed using 4-carbethoxyhexafluorobutyryl chloride. This derivatizing reagent has all the previously reported advantages of trichloroacetic anhydride (TCAA) in that it produces stable derivatives having both a higher mass fragmentation pattern and lesser volatility than derivatives of trifluoroacetic anhydride (TFAA) or heptafluorobutyric anhydride (HFBA). In addition, the assay uses deuterated internal standards for both methamphetamine and amphetamine. The procedure employs a liquid-liquid extraction and back extraction followed by acylation of the amines to their respective 4-carbethoxyhexafluorobutyramides. Excess derivatizing reagent is converted to the diethyl ester with anhydrous ethanol. At a column temperature of approximately 180 degrees C, the retention times for amphetamine and methamphetamine are 4 min and 5.5 min respectively. The monitored positive ions are: 248, 266, 294 (amphetamine); 270, 298 (amphetamine-d6); 262, 280, 308 (methamphetamine); 287, 315 (methamphetamine-d9). As a result of this high mass fragmentation pattern, which eliminates the 91 and 118 ions as criteria for both identification and quantitation, potential interferences from phentermine and phenethylamine are totally eliminated.

Authors+Show Affiliations

Navy Drug Screening Laboratory, San Diego, California 92134.No affiliation info available

Pub Type(s)

Journal Article

Language

eng

PubMed ID

2615335

Citation

Czarny, R J., and C L. Hornbeck. "Quantitation of Methamphetamine and Amphetamine in Urine By Capillary GC/MS Part II. Derivatization With 4-carbethoxyhexafluorobutyryl Chloride." Journal of Analytical Toxicology, vol. 13, no. 5, 1989, pp. 257-62.
Czarny RJ, Hornbeck CL. Quantitation of methamphetamine and amphetamine in urine by capillary GC/MS Part II. Derivatization with 4-carbethoxyhexafluorobutyryl chloride. J Anal Toxicol. 1989;13(5):257-62.
Czarny, R. J., & Hornbeck, C. L. (1989). Quantitation of methamphetamine and amphetamine in urine by capillary GC/MS Part II. Derivatization with 4-carbethoxyhexafluorobutyryl chloride. Journal of Analytical Toxicology, 13(5), 257-62.
Czarny RJ, Hornbeck CL. Quantitation of Methamphetamine and Amphetamine in Urine By Capillary GC/MS Part II. Derivatization With 4-carbethoxyhexafluorobutyryl Chloride. J Anal Toxicol. 1989 Sep-Oct;13(5):257-62. PubMed PMID: 2615335.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Quantitation of methamphetamine and amphetamine in urine by capillary GC/MS Part II. Derivatization with 4-carbethoxyhexafluorobutyryl chloride. AU - Czarny,R J, AU - Hornbeck,C L, PY - 1989/9/1/pubmed PY - 1989/9/1/medline PY - 1989/9/1/entrez SP - 257 EP - 62 JF - Journal of analytical toxicology JO - J Anal Toxicol VL - 13 IS - 5 N2 - An analytical procedure for methamphetamine and amphetamine has been developed using 4-carbethoxyhexafluorobutyryl chloride. This derivatizing reagent has all the previously reported advantages of trichloroacetic anhydride (TCAA) in that it produces stable derivatives having both a higher mass fragmentation pattern and lesser volatility than derivatives of trifluoroacetic anhydride (TFAA) or heptafluorobutyric anhydride (HFBA). In addition, the assay uses deuterated internal standards for both methamphetamine and amphetamine. The procedure employs a liquid-liquid extraction and back extraction followed by acylation of the amines to their respective 4-carbethoxyhexafluorobutyramides. Excess derivatizing reagent is converted to the diethyl ester with anhydrous ethanol. At a column temperature of approximately 180 degrees C, the retention times for amphetamine and methamphetamine are 4 min and 5.5 min respectively. The monitored positive ions are: 248, 266, 294 (amphetamine); 270, 298 (amphetamine-d6); 262, 280, 308 (methamphetamine); 287, 315 (methamphetamine-d9). As a result of this high mass fragmentation pattern, which eliminates the 91 and 118 ions as criteria for both identification and quantitation, potential interferences from phentermine and phenethylamine are totally eliminated. SN - 0146-4760 UR - https://www.unboundmedicine.com/medline/citation/2615335/Quantitation_of_methamphetamine_and_amphetamine_in_urine_by_capillary_GC/MS_Part_II__Derivatization_with_4_carbethoxyhexafluorobutyryl_chloride_ L2 - https://academic.oup.com/jat/article-lookup/doi/10.1093/jat/13.5.257 DB - PRIME DP - Unbound Medicine ER -