以GC-MS分析頭髮及頭髮片段內安非他命、甲基安非他命、MDA及MDMA成分   全文下載

Gas Chromatography-Mass Spectrometry (GC-MS) Analysis of Amphetamine, Methamphetamine, 3,4-Methylenedioxyamphetamine and 3,4-Methylenedioxymethamphetamine in Human Hair and Hair Sections

本研究建立以氣相層析質譜法同時檢測頭髮及頭髮片段內安非他命、甲基安非他命、MDA及MDMA等四種成分之分析方法。將毛髮剪成約0.5 cm之長度，經甲醇清洗後加入氘內標準品，以2 N氫氧化鈉在80℃下消化1hr，再經液相-液相萃取步驟，萃取液吹乾後以七氟丁酸酐進行衍生化，以氣相層析質譜儀分析。經評估，以50 mg空白毛髮配製濃度為2-40 ng/mg等五種不同濃度之檢體，其萃取回收率為77.45-86.86%、日間及日內精密度實驗相對標準偏差分別為0.55-7.73%及0.76-4.79%；在濃度2-40 ng/mg範圍內具有良好之線性關係，線性關係（r2）均在0.997以上；安非他命、甲基安非他命及MDMA之最低檢測極限（LOD）均在0.05 ng/mg以下，MDA在0.1 ng/mg以下；最低定量極限（LOQ）安非他命、甲基安非他命及MDMA均在0.1 ng/mg以下，而MDA在0.2 ng/mg以下。對監所內30位使用甲基安非他命觀察勒戒者之毛髮進行定量分析，結果顯示安非他命含量範圍為1.39-15.41 ng/mg，平均為5.21±3.25 ng/mg；甲基安非他命含量範圍為12.58-173.28 ng/mg，平均為56.10±36.85 ng/mg。本方法並成功應用於分段分析六位使用甲基安非他命之觀察勒戒女子之頭髮中安非他命類成分之含量檢測。本研究建立一簡單、準確與快速之方法，且已應用於例行刑事案件中頭髮內安非他命、甲基安非他命、MDA與MDMA等四種成分之檢測及定量分析。

In this paper, the authors describe a sensitive method for simultaneous quantitation of amphetamine (AM), methamphetamine (MA), 3,4-methylenedioxyamphetamine (MDA) and 3,4-methylenedioxymethamphetamine (MDMA) in human hair by gas chromatography- mass spectrometry (GC-MS). Hair samples are initially cut into 0.5-cm sections, washed with methanol, and digested for 1 hr at 80°C in 2 N NaOH and deuterated internal standards. The resulting solutions are processed with a liquid-liquid extraction procedure and further derivatized with heptafluorobutyric anhydride (HFBA) before undergoing GC/MS analysis. The overall protocol achieves the following results when applied to the analysis of 50 mg drug-free hair specimens fortified with 2-40 ng/mg amphetamines: recovery: 77.45-86.86%; inter-day and intra-day precision ranges: 0.55-7.73% and 0.76-4.79%, respectively; linearity: r2 > 0.997; detection limits: 0.05 ng/mg for AM, MA, and MDMA and 0.1 ng/mg for MDA; and quantitation limits: 0.1 ng/mg for AM, MA, and MDMA and 0.2 ng/mg for MDA. Data derived from our analysis of hair samples collected from 30 self-reported methamphetamine abusers range from 1.39 to 15.41 (mean ± S.D., 5.21 ± 3.25) ng/mg for amphetamine and 12.58 to 173.28 (mean ± S.D., 56.10 ± 36.85) ng/mg for methamphetamine. This method has also been utilized successfully to evaluate the deposition pattern of drugs in head hairs collected from six female methamphetamine abusers staying at a rehabilitation facility. We conclude that this relatively simple protocol can be used for routine and reliable identification and quantitation of AM, MA, MDA, and MDMA in hair.