固相萃取-毛细管柱-气相色谱法测定水中11种有机磷农药
Capillary Column-GC Determination of 11 Organophosphorus Pesticides in Water with Solid Phase Extraction
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摘要: 提出了固相萃取分离-毛细管柱-气相色谱法测定水中11种有机磷农药的方法。水样经Waters oasis HLB固相萃取小柱分离并净化,甲醇-丙酮(70+30)混合液洗脱。用Varian cp-sil 24CB色谱柱(30 m×0.25 mm,0.25 μm)分离,脉冲火焰光度检测器检测。11种有机磷农药的质量浓度均在5.00 μg·L-1以内与其峰面积呈线性关系,测定下限(10S/N)在0.03~0.05 μg·L-1之间。方法用于地表水样和饮用水样分析,加标回收率在65.7%~124%之间,测定值的相对标准偏差(n=6)在1.8%~9.9%之间。Abstract: Capillary GC was applied to the determination of 11 organophosphorus pesticides in water with solid phase extraction. The water sample was separated and purified by passing through Waters oasis HLB solid phase extraction column and eluted with a mixture of methanol and acetone (70+30). The eluate was separated on Varian cp-sil 24CB column (30 m×0.25 mm, 0.25 μm) and detected by PFPD. Linear relationships between values of peak area and mass concentration of the 11 organophosphorus pesticides were kept in the same range within 5.00 μg·L-1, with lower limits of determination (10S/N) in the range of 0.03-0.05 μg·L-1. The proposed method was applied to the analysis of samples of surface water and drinking water, giving values of recovery and RSD′s (n=6) in the ranges of 65.7%-124% and 1.8%-9.9% respectively.