期刊
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
卷 44, 期 2, 页码 602-607出版社
ELSEVIER
DOI: 10.1016/j.jpba.2006.12.025
关键词
pipette tip solid-phase extraction; SPE tip; methamphetamine; amphetamine; gas chromatography; mass spectrometry
Methamphetainine and amphetamine were extracted from human urine samples using pipette tip solid-phase extraction (SPE) with MonoTip C-18 tips (pipette tip volume, 200 mu l), in which C-18-bonded monolithic silica gel was fixed. A sample of human urine (0.5 ml) containing methamphetamine, amphetamine, and N-methylbenzylamine as internal standard (IS), was mixed with 25 mu l of 1M sodium hydroxide solution. The mixture was extracted into the Cis phase of the SPE tip by 25 repeated aspirating/dispensing cycles using a manual micropipettor. Analytes retained in the Cls phase were then eluted with methanol by five repeated aspirating/dispensing cycles. After derivatization with trifluoroacetic anhydride, analytes were measured by gas chromatography/mass spectrometry with selected ion monitoring in the positive-ion electron impact mode. Recoveries of methamphetamine, amphetamine, and IS spiked into urine were more than 82.9, 82.2, and 78.2%, respectively. Regression equations for methamphetamine and amphetamine showed excellent linearity in the range of 0.25-200 ng/0.5 ml. Limit of detection was 0.04 ng/0.5 ml for methamphetamine and 0.05 ng/0.5 ml for amphetamine. Intra- and inter-day coefficients of variations for both stimulants were not greater than 10.8%. The data obtained from actual determination of methamphetamine and amphetamine in autopsy urine samples are also presented for validation of the method.
作者
我是这篇论文的作者
点击您的名字以认领此论文并将其添加到您的个人资料中。
推荐
暂无数据