顶空固相微萃取-气相色谱质谱联用测定烷基铅的研究

Study of alkyllead speciation by HS-SPME coupled with GC/MS

建立了顶空固相微萃取(HS SPME)与气相色谱 质谱(GC/MS)联用测定水样中四甲基铅和四乙基铅的方法,探讨了SPME萃取烷基铅的实验条件,并对GC/MS条件进行了优化。结果表明:四甲基铅和四乙基铅分别在5～1000ng/mL和1～500ng/mL范围内有良好的线性关系,检出限分别为四甲基铅5.19ng/mL,四乙基铅1.05ng/mL。方法用于合成水样分析,四甲基铅和四乙基铅的回收率在87.5%～110.6%之间,相对标准偏差在1.7%～6.5%之间。

A method of head space solid phase microextraction(HS-SPME) coupled with gas chromatography-mass spectrometry for the determination of tetramethyllead and tetraethyllead in water sample was developed. The conditions of SPME extraction and GC-MS determination were discussed. The linear range of determination of tetramethyllead and tetraethyllead was 5～1000 ng/mL with a detection limit of 5.2 ng/mL, 1～500 ng/mL with a detection limit of 1.1 ng/mL, respectively. The average recoveries of tetramethyllead and tetraethyllead in water were in the range of 87.5%～110.6%.