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    液液萃取处理样品-气相色谱法测定水中22种有机氯农药

    GC Determination of 22 Organochlorine Pesticides in Water with Pretreatment of Samples by Liquid-liquid Extraction

    • 摘要: 采用正己烷作萃取溶剂提取并富集水样中有机氯农药(OCP),所得提取液经浓缩并定容为1.0 mL后,用气相色谱法-电子捕获检测器测定22种有机氯农药.采用Rtx-CLP Ⅱ和Rtx-1701双柱法根据与标准物质的保留时间相比较进行定性;采用Rtx-CLP Ⅱ柱对被测组分按外标法进行定量.结果表明:各种农药质量浓度在1~80 μg·L-1范围内与峰面积呈线性关系.22种有机氯农药的方法检出限(3S/N)在1.5~5.6 ng·L-1之间.用标准加入法测得其回收率在73.3%~107.9%之间,相对标准偏差(n=7)在2.9%~14.8%之间.

       

      Abstract: Gas chromatography with electron capture detector was applied to simultaneous determination of 22 organochlorine pesticides (OCP′s) in water.OCP′s was separated and enriched from the water sample by extraction with n-hexane.The extract was concentrated and diluted to 1.0 mL with n-hexane.The double capillary chromatographic column practice,i.e.use of 2 columns of different polarity (the Rtx-CLP Ⅱ column and the Rtx-1701 column) was adopted for identification of the OCP′s by comparing values of tR with reference materials,and quantification of the OCP′s was performed by using the Rtx-CLP Ⅱ column with external standard method.Linear relationships between values of peak area and mass concentration of the 22 OCP′s were found same in the range of 1-80 μg·L-1,with detection limits (3s/k) in the range of 1.5-5.6 μg·L-1.Recovery of the method was tested,giving values of average recovery ranged from 73.3% to 107.9% and RSD′s (n=7) ranged from 2.9% to 14.8%.

       

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