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优化了C18固相膜萃取条件,建立了C18膜萃取-气相色谱/质谱联用测定海螺沟冰雪中16种多环芳烃的分析方法。结果表明,C18圆盘萃取减少了提取时间、提高了萃取效率、节省了试剂,还可以加大取样量。采用GC/MS的选择离子检测方式对分别加有高、中、低三种浓度混标的3 L纯水中PAHs进行定性定量分析,测得相对标准偏差小于15.83%,平均回收率分别为75.98%~99.30%、79.50%~91.60%和76.31%~89.78%,方法检出限为0.001 0~0.010 7μg/L。将本方法应用于海螺沟雪水的检测,结果满足其冰雪中多环芳烃的分析要求。
The extraction conditions of C18 solid-phase membrane were optimized and the determination method of 16 polycyclic aromatic hydrocarbons (PAHs) in ice and snow of Hailuogou by C18 membrane extraction-gas chromatography / mass spectrometry was established. The results showed that C18 disk extraction reduced the extraction time, increased the extraction efficiency, saved the reagent, and increased the sample volume. The selective ion detection method of GC / MS was used to qualitatively and quantitatively analyze the PAHs in 3 L pure water mixed with high, medium and low concentration respectively, the relative standard deviation was less than 15.83% and the average recovery was 75.98% ~ 99.30%, 79.50% ~ 91.60% and 76.31% ~ 89.78%, respectively. The detection limits were 0.001 0 ~ 0.010 7 μg / L. Applying this method to the detection of snow water in Hailuogou, the results meet the analytical requirements of PAHs in ice and snow.