富氮多孔有机聚合物包覆SPME探针用于生物样品中甲基苯丙胺的检测及灵敏度分析

The sensitive detection of methamphetamine in biological samples based on a nitrogen-rich porous organic polymer modified SPME Probe

目的设计制备富氮多孔有机聚合物功能化固相微萃取探针用于生物样本中甲基苯丙胺的快速分析与检测。方法将一种三聚氰胺改性的富氮多孔有机聚合物作为涂层制备出固相微萃取探针,优化萃取条件,富集生物样本中的甲基苯丙胺,用气相色谱-质谱(GC-MS)分析检测。结果在提取时间25 min,洗脱溶剂丙酮,洗脱时间1 min,洗脱剂体积1 mL的最优条件下建立的方法在5~5000 ng/mL的范围内呈良好线性关系(R^(2)=0.999,n=7),甲基苯丙胺的检测限为0.35 ng/mL,定量限为1.02 ng/mL,在低、中、高(100、500、1000 ng/mL)浓度的加标平均相对回收率为83.5%~112.1%,RSD均小于6%。结论本文成功制备了一种富氮多孔有机聚合物功能化固相微探针,结合气相色谱质谱技术建立了生物样本中甲基苯丙胺测定的新方法,该方法灵敏度高,简单快捷,可用于实际样本的快速定性定量检测。

Objective Design and preparation of a new nitrogen-rich porous organic polymer-functionalized solid-phase microextraction probe for rapid analysis and detection of methamphetamine in biological samples.Methods A SPEM-GC-MS method was estabished for detection of methamphetamine in biological samples,employing a melamine-modified nitrogen-rich porous organic polymer functionalized solid-phase microextraction probe.The extraction conditions were optimized.Results The results demonstrated that the optimal conditions included the extraction time of 25 min,elution solvent of acetone,desorption time of 1 min,and optimal elution volume of 1 mL.Under the optimized conditions,the method exhibited good linearity within the range of 5 to 5000 ng/mL(R^(2)=0.999,n=7).The detection limit and quantification limit were 0.35 ng/mL and 1.02 ng/mL respectively.The spiked recoveries at low,medium and high concentrations(100,500,1000 ng/mL)ranged from 83.5%to 112.1%,with the relative standard deviations(RSD,n=3)than 6%.Conclusion A nitrogen-rich solid phase microprobe was prepared,functionalized with porous organic polymer.The SPME-GC-MS method was established for high sensitivity,simple,and rapid detection of methamphetamine in biological samples.This method can be utilized for rapid qualitative and quantitative detection of real samples.