Luo Dan, Chen Fei, Xiao Kuang, Feng Yu-Qi
Department of Chemistry, Wuhan University, Wuhan 430072, PR China.
Talanta. 2009 Mar 15;77(5):1701-6. doi: 10.1016/j.talanta.2008.10.007. Epub 2008 Oct 17.
A method was developed for the determination of Delta(9)-Tetrahydrocannabinol (THC) in saliva by polymer monolith microextraction (PMME) combined with gas chromatography-mass spectrometry. The poly(methacrylic acid-co-ethylene glycol dimethacrylate) (p(MAA-co-EGDMA)) monolithic capillary column was selected as the extraction medium of PMME, which showed high extraction capacity towards THC in saliva. To reach optimum PMME extraction performance, several PMME parameters were investigated, including matrix pH, flow rate for extraction, sampling volume and elution solvent. Under the optimal conditions, good extraction efficiency was obtained with no matrix interference in the process of extraction and the subsequent GC-MS analysis. In the selected-ion monitoring (SIM) mode, the limit of detection (LOD) for THC was 0.68 ng/mL. The linearity range of the method was 3-300 ng/mL. Excellent reproducibility of the method was exhibited by intra- and inter-day precisions, yielding the relative standard deviations (R.S.D.s) less than 12%; recoveries higher than 89%. The proposed method was proved to be rapid, sensitive, and competently applied to the determination of THC in saliva samples.
建立了一种采用整体柱微萃取(PMME)结合气相色谱-质谱联用技术测定唾液中Δ⁹-四氢大麻酚(THC)的方法。选用聚(甲基丙烯酸-co-乙二醇二甲基丙烯酸酯)(p(MAA-co-EGDMA))整体柱毛细管柱作为PMME的萃取介质,该介质对唾液中的THC具有较高的萃取能力。为达到最佳的PMME萃取性能,研究了几个PMME参数,包括基质pH值、萃取流速、进样体积和洗脱溶剂。在最佳条件下,萃取效率良好,萃取过程及后续气相色谱-质谱分析中无基质干扰。在选择离子监测(SIM)模式下,THC的检测限(LOD)为0.68 ng/mL。该方法的线性范围为3-300 ng/mL。日内和日间精密度表明该方法具有出色的重现性,相对标准偏差(R.S.D.s)小于12%;回收率高于89%。所提出的方法被证明快速、灵敏,适用于唾液样品中THC的测定。