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|標題:||Orthogonal array optimization of microwave-assisted derivatization for determination of trace amphetamine and methamphetamine using negative chemical ionization gas chromatography-mass spectrometry||作者:||Chung, L.W.
|關鍵字:||Analysis of variance;Gas chromatography-mass spectrometry;Microwave-assisted derivatization;Negative chemical ionization;Orthogonal array design;carbon-dioxide extraction;solid-phase extraction;quantitative-determination;hair analysis;urine;performance;ketamine;samples;design;pharmacokinetics||Project:||Journal of Chromatography A||期刊/報告no：:||Journal of Chromatography A, Volume 1216, Issue 18, Page(s) 4083-4089.||摘要:||
An orthogonal array design (OAD) was applied to optimize microwave-assisted derivatization (MAD) for analysis of trace amphetamine (AM) and methamphetamine (MA) by negative chemical ionization gas chromatography-mass spectrometry (NCI GC-MS). The 2,3,4,5,6-pentafluorobenzoyl chloride (PFBC) was used as a derivatization reagent. Experimental factors including solvent, microwave power, and irradiation time at four-levels were studied in 16 trials by OAD(16) (4(4)). The significance of these factors was investigated using analysis of variance (ANOVA) and percent contribution (PC). Solvent is statistically demonstrated a chief factor; microwave power and irradiation time are secondary factors. Under the optimum condition, calibration curve of AM is linear over a range from 0.01 to 100 ng mL(-1) with correlation coefficient 0.9988, and MA from 0.1 to 1000 ng mL-1 with correlation coefficient 0.9951. The limit of detection (LOD) is 1.20 pg mL(-1) for AM and 13.04 pg mL(-1) for MA. An applicability of the method was tested by analyzing urine samples from amphetamine-type stimulants (ATS)-abusing suspects. Consequently, the CAD method not only optimizes the MAD condition for determination of trace AM and MA,but identifies the effects of factor solvent, microwave power and irradiation time on the MAD performance. (C) 2009 Elsevier B.V. All rights reserved.
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