固相微萃取-气相色谱-质谱法测定水中双酚A

Determination of Bisphenol A in Water by Solid Phase Microextracion Coupled with Gas Chromatography-Mass Spectrometry

基于固相微萃取技术 (SPME)具有前处理方法操作简单、避免使用有机溶剂、回收率高等优点 ,且容易与其它分析仪器联用 ,建立了一种顶空衍生固相微萃取 -气相色谱 -质谱法 (SPME-GC/MS)测定水中双酚 A的分析方法。通过优化 SPME纤维头、萃取温度和时间、解吸时间、搅拌速度、p H值等萃取条件及衍生化温度和衍生化时间等衍生化条件 ,实现了水中痕量双酚 A的快速测定。结果表明 :用 85 μm的聚丙烯酸酯 (PA)萃取涂层对水中的双酚 A萃取效果很好 ,双酚 A在 0 .0 1～ 1 0 0 μg/L的质量浓度范围内 ,线性良好 ,相关系数 >0 .999,方法的检测限为 2 .5 ng/L (S/N =3 ) ,相对标准偏差 (n=7)为 3 .1 3 % ,回收率为 86.3 %～ 95 .6%。

A new method for the determination of bisphenol A in water has been established by coupling solid-phase microextraction (SPME) with gas chromatography-mass spectrometry because of SPME with the characteristics of simple pretreatment procedure without organic, high recovery rate and easy to be coupled with other analytical instruments. Through optimizing extraction and derivatization conditions of SPME, such as fibers, extraction temperature and extraction time, desorption time, stirring rate, pH value, derivatization temperature and derivatization time, the rapid determination of trace bisphenol A in water was performed. The results showed that a SPME fiber with 85μm polyacrylate coated was used to extract bisphenol A from water with satisfactory results. The linear ranges of bisphenol A were from 0.01μg/L to 100μg/L, the relative coefficient was above 0.999. The detection limits and the relative standard deviation were 2.5ng/L (S/N=3) and 3.13%, respectively. The recovery were from 86.3% to 95.6%.