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    顶空-固相微萃取-气相色谱法测定水蜜桃中有机氯农药

    GC Determination of 11 Organochlorine Pesticides in Honey Peaches with Separation by HS-SPME

    • 摘要: 应用顶空-固相微萃取分离、富集,气相色谱法测定了水蜜桃中11种有机氯农药。称取匀浆后的果浆样品5.000 g,加水15 mL稀释。取此样品溶液2.00 mL置于12 mL安瓿瓶中,加入氯化钠1.0 g,放入搅拌子后将瓶盖紧,置于70 ℃水浴中。将聚二甲基硅氧烷萃取头插入瓶中,置于离试样液面1.0 cm的顶空处,在600 r·min-1搅拌速率下萃取30 min。萃取完成后,将萃取头从瓶中抽出并直接插入色谱仪的进样口,热解吸5 min。被测组分随载气进入SE-54石英毛细管柱进行分离,用电子捕获检测器检测。11种有机氯农药在一定浓度范围内与相应峰面积呈线性关系,检出限(3S/N)在1.33~42.3 ng·kg-1之间。对方法的回收率和重复性进行试验,测得回收率在90.6%~112%之间,测定值的相对标准偏差(n=5)均小于10%。

       

      Abstract: GC with separation and enrichment by HS-SPME was applied to the determination of 11 organochlorine pesticides (OCP′s). 5.000 g of the fruit pulp were taken and diluted with 15 mL of H2O. An aliquot of 2.00 mL was placed into a 12 mL ampoule and added with 1.0 g of NaCl. After capping the ampoule tightly, it was placed into a water bath at 70 ℃. A PDMS extractor was inserted into the ampoule with its injector placed at 1.0 cm over the solution level in the head-space. SPE was carried out with stirring at the rate of 600 r·min-1 for 30 min. The extractor was removed from the ampoule and inserted directly into the sample inlet of the chromatograph for thermo-desorption. After desorption for 5 min, the analytes were carried by carrier gas to pass through SE-54 quartz capillary chromatographic column for separation and measured with ECD. Linearities in definite concentration ranges were kept for the 11 OCP′s, and detection limits (3S/N) in the range of 1.33-42.3 ng·kg-1 were found. Recovery and repeatability were tested, giving values of recovery ranged from 90.6% to 112%, and RSD′s (n=5) all less than 10%.

       

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