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采用电泳微芯片与非接触式电导检测集成的方法测定饮料、尿液和 Buscopan®片剂样品中的莨菪碱和丁基莨菪碱。

Determination of scopolamine and butylscopolamine in beverages, urine and Buscopan® tablets samples using electrophoresis microchip with integrated contactless conductivity detection.

机构信息

Instituto de Química, Universidade Federal de Goiás, 74690-900, Goiânia, GO, Brazil.

Instituto de Química, Universidade Federal de Uberlândia, 38408-100, Uberlândia, MG, Brazil; Instituto Nacional de Ciência e Tecnologia de Bioanalítica, 13084-971, Campinas, SP, Brazil.

出版信息

Talanta. 2024 Jan 1;266(Pt 1):124960. doi: 10.1016/j.talanta.2023.124960. Epub 2023 Jul 17.

DOI:10.1016/j.talanta.2023.124960
PMID:37487267
Abstract

The number of cases in which scopolamine (SCO) was used for both recreational and predatory purposes has increased dramatically in recent decades. Linked to this, there is a concern about obtaining SCO through thermal degradation of butylscopolamine (BSCO) - an active ingredient of Buscopan® - a drug sold without a medical prescription. In this study, mixtures containing SCO and BSCO were separated and detected on a microchip electrophoresis (ME) device with integrated capacitively coupled contactless conductivity detection (CD) using a running buffer composed of 40 mmol L of butyric acid and 25 mmol L of sodium hydroxide (pH 5.0). The separation was performed within ca. 115 s with a resolution of 1.3 and separation efficiency ranging from 1.4 × 10 to 1.5 × 10 theoretical plates m. A detection limit of 1.1 μmol L was achieved for both species and the developed method revealed satisfactory repeatability with relative standard deviation (RSD) values for forty-eight injections between 4.8 and 9.4% for peak areas and lower than 3.3% for migration times. Furthermore, inter-day precision was evaluated for sixteen injections (a sequence of four injections performed over four days), and RSD values were less than 6.6% for peak areas and 2.2% for migration times. Satisfactory recovery values (95-114%) were obtained for all evaluated beverage samples (cachaça, vodka, whiskey, beer, Coca-Cola, and grape juice) as well as for artificial urine samples (95-107%). Finally, the conversion of BSCO into SCO was observed after simple heating procedure of Buscopan® sample (not subject to medical prescription), which was successfully confirmed through analysis by capillary electrophoresis coupled to the mass spectrometry (CE-MS). Based on the reported results, the use of ME-CD devices has demonstrated a huge potential for applications in the forensic chemistry field.

摘要

近年来,莨菪碱(SCO)被用于娱乐和掠夺性目的的案例数量急剧增加。与此相关的是,人们担心通过热降解丁基莨菪碱(BSCO)——一种无处方销售的药物 Buscopan®的有效成分——来获得 SCO。在这项研究中,使用含有 40mmol/L 丁酸和 25mmol/L 氢氧化钠(pH 5.0)的运行缓冲液,在带有集成电容耦合非接触式电导检测(CD)的微芯片电泳(ME)设备上分离和检测含有 SCO 和 BSCO 的混合物。分离在约 115s 内完成,分辨率为 1.3,分离效率在 1.4×10 到 1.5×10 理论板 m 之间。两种物质的检测限均达到 1.1μmol/L,所开发的方法显示出令人满意的重复性,48 次进样的峰面积和迁移时间的相对标准偏差(RSD)值分别为 4.8%至 9.4%和低于 3.3%。此外,对 16 次进样(在四天内进行四次进样的序列)进行了日间精密度评估,峰面积的 RSD 值小于 6.6%,迁移时间的 RSD 值小于 2.2%。所有评估的饮料样品(甘蔗酒、伏特加、威士忌、啤酒、可口可乐和葡萄汁)以及人工尿液样品(95-107%)均获得了令人满意的回收率(95-114%)。最后,在简单加热 Buscopan®样品(无需处方)后观察到 BSCO 转化为 SCO,这通过毛细管电泳与质谱(CE-MS)分析成功得到证实。基于报告的结果,ME-CD 设备在法医化学领域的应用具有巨大的潜力。

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