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采用高效液相色谱三重四极杆质谱联用技术(LC-MS/MS)检测毛发样本中的 1-苄基哌嗪(BZP)的定量分析。

Quantitative analysis of hair samples for 1-benzylpiperazine (BZP) using high-performance liquid chromatography triple quadrupole mass spectrometry (LC-MS/MS) detection.

机构信息

Kenepuru Science Centre, Institute of Environmental Science and Research Ltd, Porirua, New Zealand.

出版信息

Anal Bioanal Chem. 2011 Oct;401(6):2013-7. doi: 10.1007/s00216-011-5235-5. Epub 2011 Jul 15.

Abstract

Benzylpiperazine (BZP) is an amphetamine-type stimulant, which was legally available in New Zealand and widely used in "Party Pills" until reclassification as a Class C drug in April 2008. BZP was included as part of a multi-analyte method developed for hair screening using high-performance liquid chromatography triple quadrupole mass spectrometry (LC-MS/MS). A 20-mg sample of hair is extracted and partially purified using mixed-mode solid-phase extraction cartridges prior to analysis by LC-MS/MS. The method was developed as a broad screen for drugs of abuse (including amphetamines, opiates, and benzodiazepines), with only the BZP results being presented here. The assay was validated and found to be linear over the range of 0.085 to 8.65 ng/mg with correlation coefficient of r (2) ≥ 0.99. Blank hair samples spiked with BZP at 0.22 and 2.16 ng/mg gave intra- and inter-day precision coefficients of variation of ≤10% (n = 6 per day, 3 days) at both levels and calculated extraction efficiencies of 78% and 91%, respectively. The results from the samples submitted to the laboratory for BZP analysis showed 11% were positive (n = 126). The mean BZP level was 3.9 ng/mg (range, 0.4-33 ng/mg; the result was extrapolated when above the calibration). These data are the first available showing the levels expected from users of BZP.

摘要

苯甲哌嗪(BZP)是一种苯丙胺类兴奋剂,在 2008 年 4 月被重新归类为 C 类药物之前,在新西兰合法销售,并广泛用于“派对药丸”中。BZP 被纳入一种多分析物毛发筛查方法中,该方法使用高效液相色谱三重四极杆质谱联用仪(LC-MS/MS)。取 20mg 毛发样本,使用混合模式固相萃取小柱进行提取和部分纯化,然后进行 LC-MS/MS 分析。该方法是一种广泛用于筛查滥用药物(包括苯丙胺类、阿片类和苯二氮䓬类)的方法,这里仅呈现 BZP 的结果。该检测方法已通过验证,发现其在 0.085 至 8.65ng/mg 范围内呈线性关系,相关系数 r(2)≥0.99。在 0.22 和 2.16ng/mg 两个浓度水平下,空白毛发样品分别加入 BZP 后,日内和日间精密度变异系数(CV)均≤10%(每天 6 个样本,共 3 天),计算得出的提取效率分别为 78%和 91%。提交给实验室进行 BZP 分析的样本中,有 11%为阳性(n=126)。BZP 的平均水平为 3.9ng/mg(范围为 0.4-33ng/mg;当结果超过校准范围时进行外推)。这些数据是首次提供的关于 BZP 用户预期水平的可用数据。

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