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用于甲基苯丙胺和苯丙胺测定的强化毛发标准物质的制备与应用

Preparation and application of a fortified hair reference material for the determination of methamphetamine and amphetamine.

作者信息

Lee Sooyeun, Park Yonghoon, Han Eunyoung, Choe Sanggil, Lim Miae, Chung Heesun

机构信息

National Institute of Scientific Investigation, 331-1 Sinwol-7-dong, Yangcheon-gu, Seoul 158-707, South Korea.

出版信息

Forensic Sci Int. 2008 Jul 4;178(2-3):207-12. doi: 10.1016/j.forsciint.2008.04.005. Epub 2008 May 23.

DOI:10.1016/j.forsciint.2008.04.005
PMID:18502069
Abstract

Quality assurance is one of the major issues in forensic analytical laboratories, where the need for a reference material (RM) has rapidly increased. RMs are very useful for method development and validation, internal quality control or proficiency tests. In the present study, we prepared a RM using drug-free hair for the determination of methamphetamine (MA) and its main metabolite, amphetamine (AP) according to the recommendations of ISO Guide 35. The concentrations of MA and AP were determined using two extraction methods, agitation with 1% HCl in methanol at 38 degrees C and ultrasonication with methanol/5M HCl (20:1), followed by gas chromatography/mass spectrometry (GC/MS) after derivatization with trifluoroacetic anhydride (TFAA). The assignment of values was conducted through the homogeneity study and characterization of the material. Furthermore, an internal proficiency test was performed with the prepared RM, of which the results were compared with those of the authentic hair RM prepared in our previous study. As a result, a hair RM containing MA and AP was prepared at the level of 4.86+/-0.69 ng/mg and 4.63+/-0.44 ng/mg, respectively. Most participants showed satisfactory performances in the internal proficiency test with the both RMs. The hair RM prepared in this study demonstrated its suitability for quality assurance in forensic laboratories.

摘要

质量保证是法医分析实验室的主要问题之一,在这些实验室中,对参考物质(RM)的需求迅速增加。参考物质对于方法开发与验证、内部质量控制或能力验证测试非常有用。在本研究中,我们根据ISO指南35的建议,使用不含药物的毛发制备了一种参考物质,用于测定甲基苯丙胺(MA)及其主要代谢物苯丙胺(AP)。采用两种提取方法测定MA和AP的浓度,一种是在38℃下用1%盐酸甲醇溶液振荡提取,另一种是用甲醇/5M盐酸(20:1)超声提取,然后用三氟乙酸酐(TFAA)衍生化后进行气相色谱/质谱(GC/MS)分析。通过材料的均匀性研究和特性表征来赋值。此外,用制备的参考物质进行了内部能力验证测试,并将结果与我们之前研究中制备的真实毛发参考物质的结果进行了比较。结果,制备了一种含有MA和AP的毛发参考物质,其含量分别为4.86±0.69 ng/mg和4.63±0.44 ng/mg。大多数参与者在使用这两种参考物质的内部能力验证测试中表现令人满意。本研究中制备的毛发参考物质证明了其适用于法医实验室的质量保证。

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