Department of Chemistry, Faculty of Science, Shinshu University, 3-1-1 Asahi, Nagano 390-8621, Japan.
Research Institute of Scientific Criminal Investigation, Nagano Prefectural Police Headquarters, 3916 Nishijo, Matsushiro, Nagano 381-1232, Japan.
Molecules. 2018 Dec 7;23(12):3231. doi: 10.3390/molecules23123231.
A simple, sensitive, and rapid extraction method based on high-frequency (H-F) heating was developed for drug analysis in human nails. A human nail was placed in a glass tube with an extraction solvent (methanol and 0.1% formic acid; 7:3, /), and a ferromagnetic alloy (pyrofoil) was wrapped in a spiral around the glass tube. Then, the glass tube was placed in a Curie point pyrolyzer, and a H-F alternating voltage (600 kHz) was applied. The sample and extraction solvent were heated at the Curie temperature for 3 min. Different Curie temperatures were applied by changing the pyrofoil (160 °C, 170 °C, 220 °C, and 255 °C). The caffeine in the nail was effectively and rapidly extracted into the extraction solvent with the pyrofoil at 220 °C. The peak area obtained for the caffeine using liquid chromatography mass spectrometry (LC-MS/MS) was five times that of what was obtained after conventional ultrasonic irradiation extraction. Because the extraction uses high-pressure and high-temperature conditions in a test tube, the drugs that were strongly incorporated in nails could be extracted into the solvent. The amount of caffeine extracted was independent of the size of the pieces in the sample. Therefore, the sensitive determination of target drugs in nails is possible with rapid (20 min, including H-F extraction for 3 min) and simple sample preparation. The developed method was applied to a nail from a patient with hypertension.
基于高频(H-F)加热的简单、灵敏、快速提取方法已被开发用于人指甲中的药物分析。将人指甲放入装有提取溶剂(甲醇和 0.1%甲酸;7:3,/)的玻璃管中,并用铁磁合金(Pyrofoil)螺旋缠绕在玻璃管周围。然后,将玻璃管放入居里点热解仪中,并施加 H-F 交流电压(600 kHz)。样品和提取溶剂在居里温度下加热 3 分钟。通过改变 Pyrofoil(160°C、170°C、220°C 和 255°C)来应用不同的居里温度。用 220°C 的 Pyrofoil 可将指甲中的咖啡因有效且快速地提取到提取溶剂中。使用液相色谱质谱法(LC-MS/MS)获得的咖啡因峰面积是常规超声辐照提取后获得的咖啡因峰面积的五倍。由于提取在试管中使用高压和高温条件,因此可以将强烈结合在指甲中的药物提取到溶剂中。提取的咖啡因量与样品中碎片的大小无关。因此,通过快速(20 分钟,包括 3 分钟的 H-F 提取)和简单的样品制备,可以对指甲中的目标药物进行灵敏测定。所开发的方法已应用于高血压患者的指甲。