| Abstrakt: |
Recently, certain laboratories reported the presence of methamphetamine in several negative urine specimens. We have demonstrated an artifact peak, by SIM GC/MS, in negative urine specimens, that frequently matches the retention time and identity ion ratio criteria for methamphetamine. This peak resulted from the presence of high levels of pseudoephedrine (PS) or ephedrine (EP) and was produced after derivatization with 4-carbethoxyhexafluorobutyryl chloride (CB), heptafluorobutyric anhydride (HFB), and N-trifluoroacetyl-l-prolyl chloride (TFAP). Use of N-methyl trideuterated PS and two deuterated EP compounds in spiked samples provided additional proof that PS and EP can produce the artifact peak. The above results were achieved using a GC injection port temperature of 300 degrees C and low split and isothermal conditions. Thermal transformation in the injector is involved because lowering and raising the injector temperature results in the disappearance and subsequent reappearance of the artifact peak. Proof that the artifact peak is actually methamphetamine was provided by full-scan GC/MS data of the artifact peak produced after use of all three derivatizing reagents. GC/MS analysis has demonstrated that urine (65 specimens) with concentrations of PS or EP ranging from 100,000 to 1,100,000 ng/mL will test negative for methamphetamine, while the same specimens will trigger positive results by radioimmunoassay and the Emit monoclonal assay. Full-scan GC/MS of the CB derivative for PS and EP reveals what appears to be both mono- and diderivatized products. SIM analysis can differentiate between PS and EP in urine specimens because the relative amounts of mono- and diderivatized products are very different for PS than for EP.(ABSTRACT TRUNCATED AT 250 WORDS) |
