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.

中文翻译：

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用壳聚糖纳米复合材料与聚氧杂双酸纳米团簇/氧化石墨烯结合固相微萃取美沙酮

在本研究中，我们报告了由壳聚糖/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，及其在顶空固相微萃取结合离子迁移谱法分析生物基质中美沙酮的应用. 通过红外光谱和热重分析对开发的纳米复合材料进行了表征。由于其大比表面积，三元纳米复合涂层具有良好的机械和热稳定性以及高提取效率。使用中心复合统计设计来研究影响提取效率的主要变量。然后，为了研究不同输入和输出变量之间的关系以及确定最佳操作条件，使用响应面方法，通过二阶多项式方程拟合实验数据。优化提取条件为：温度，70℃；萃取时间，15 分钟；和 NaCl 浓度，5%w/v。在优化的提取条件下获得了 0.12 ng/mL 的检出限，校准曲线在 0.30–200 ng/mL 的浓度范围内呈线性。该方法检测限相对较低，精密度好，具有用于生物样品中美沙酮的提取和测定的潜力。校准曲线在 0.30–200 ng/mL 的浓度范围内呈线性。该方法检测限相对较低，精密度好，具有用于提取和测定生物样品中美沙酮的潜力。校准曲线在 0.30–200 ng/mL 的浓度范围内呈线性。该方法检测限相对较低，精密度好，具有用于提取和测定生物样品中美沙酮的潜力。