Department of Police Equipment and Technologies, Police Sciences and Social Studies Institute, Tehran, Iran.
J Sep Sci. 2021 May;44(9):1969-1977. doi: 10.1002/jssc.202100095. Epub 2021 Mar 19.
In the present study, we report on the simple sol-gel preparation of a nanocomposite composed of chitosan/ polyoxometalate /graphene oxide, and its application in the headspace solid-phase microextraction combined with the ion mobility spectrometry for the analysis of methadone in biological matrices. The developed nanocomposite was characterized through the infrared spectroscopy and thermogravimetric analyses. The ternary nanocomposite coating offers good mechanical and thermal stability and high extraction efficiency thanks to its large specific surface. A central composite statistical design was used to study the main variables affecting the extraction efficiency. Afterward, to study the relationship between different input and output variables as well as to identify the optimal operating conditions, response surface methodology was used, whereby a second-order polynomial equation was fit to the experimental data. The optimized extraction conditions were as follows: temperature, 70°C; extraction time, 15 min; and concentration of NaCl, 5%w/v. The detection limit of 0.12 ng/mL was obtained at the optimized extraction conditions, and the calibration plot was linear in the concentration range of 0.30-200 ng/mL. With relatively low limit of detection and good precisions, the proposed method has the potential for the extraction and determination of methadone in biological samples.
在本研究中，我们报告了一种由壳聚糖/多金属氧酸盐/氧化石墨烯组成的纳米复合材料的简单溶胶-凝胶制备方法，并将其应用于顶空固相微萃取与离子淌度谱联用分析生物基质中的美沙酮。所开发的纳米复合材料通过红外光谱和热重分析进行了表征。由于其大的比表面积，三元纳米复合材料涂层具有良好的机械和热稳定性以及高的萃取效率。采用中心复合统计设计研究了影响萃取效率的主要变量。然后，为了研究不同输入和输出变量之间的关系并确定最佳操作条件，使用响应面法对实验数据进行拟合，得到一个二次多项式方程。优化的萃取条件如下：温度 70°C；萃取时间 15 分钟；NaCl 浓度 5%w/v。在优化的萃取条件下，检测限为 0.12ng/mL，校准曲线在 0.30-200ng/mL 浓度范围内呈线性。该方法具有较低的检测限和良好的精密度，有望用于生物样品中美沙酮的提取和测定。
