分散液-液微萃取结合离子迁移谱测定人体唾液中的苯海拉明

建立一种结合便携式高分辨离子迁移谱(IMS)快速简便萃取唾液中的苯海拉明(DPH)的分散液-液微萃取法(DLLM E)。取2 mL唾液,采用10%(w:V)硫酸锌沉淀蛋白,以2 mL二氯甲烷为萃取剂对唾液中的苯海拉明进行萃取,萃取时间5 min,离心(3500 r/min,20 min),取二氯甲烷层,45℃真空干燥,甲醇复溶后进行IMS分析。结果表明,该方法可在短时间内完成对DPH的萃取分离及分析,DPH在39.4~1080 ng/mL范围内线性关系良好,标准曲线方程为I=3.62×10³-0.754(R²=0.978),检出限和定量限分别为11.8和39.4 ng/mL,平均回收率为89.0%~112%,RSD≤1.5%。该方法可实现对人体唾液中苯海拉明的快速测定。

Dispersive liquid-liquid microextraction combined with ion mobility spectrometry for determination of diphenhydramine in human saliva

A quick and simple dispersive liquid-liquid microextraction(DLLME)method was established to extract the diphenhydramine(DPH)in saliva followed by portable high-resolution ion mobility spectrometry(IMS)detection.2 m L saliva was collected and the protein was firstly precipitated by 10%ZnSO4,then DPH in saliva was extracted by 2 m L dichloromethane.The extraction time was 5 min.After centrifugation at 3500 r/min for20 min,the dichloromethane layer was taken and dried in vacuum at 45℃.Then the residue was dissolved in methanol for IMS analysis.The results showed that the separation and analysis of DPH was achieved in a short time.The DPH had a good linear relationship in the range of 39.4~1080 ng/m L,the standard curve equation was I=3.62×10³ C-0.754(R²=0.978),the limit of detection and limit of quantitation were 11.8 and39.4 ng/m L,respectively.The average recovery was 89%-112%with RSD≤1.5%.This method can be used for rapidly determination of DPH in human saliva.