花粉中有机氯类农药串联固相萃取柱净化--气相色谱分析

本文旨在研究应用气相色谱一电子俘获检测器（GC—ECD）测定花粉中17种有机氯农药（OCPS）残留的检测方法。样品经丙酮／正己烷（V/V，1：1）浸泡过夜并超声提取后，研究了两种固相萃取柱（SPE）对样品的净化效果。结果表明：单独使用弗洛里硅土柱能获得满意的回收率，但基质干扰多。弗洛里硅土柱与石墨化碳柱联用能够取得更好的回收率和无色洗脱。在线性范围为0．005-5mg／L时，所有的有机氯农药都呈现很好的线性，相关系数均大于0．99。方法的检出限范围是0．81～1．99，定量限为2．64巧．62。在空白花粉样品中添加0．1mg／L、0．05mg／L的有机氯农药浓度水平下，茶花和油菜都得到了满意的回收率，平均回收率范围是60．6％-115．9％，相对标准偏差为1．2％-13．1％。实际样品的测定表明，污染严重的底泥在一定程度上影响了荷花粉的质量安全。

Determination of organochlorine pesticides in pollen by gas chromatography- electron capture detection using double column series solid-phase extraction

A method for simultaneous determination of 17 organochlorine pesticides （OCPs） in pollen by gas chromatography with electron capture detection （GC-ECD） was described in our research. The sample was saturated with hexane and acetone （1：1, V/V） overnight and extracted by ultrasonic. Two sorbents （florisil, graphitized carbon plus florisil） were assayed for the clean-up step. The results showed good recoveries were also achieved by using single florisil cartridge, but more interference than tandem graphitized carbon and florisil cartridge, which gave a colorless eluates. The correlation coefficients of linear regression for analyzed concentration （5-500 ug/kg） were all 〉0.99. The limits of detection （LODs） varied between 0.81 ug/kg and 1.99 ug/kg,and limit of quantitation （LOQs） ranged from 2.64 to 6.62 ug/kg. The average recoveries were satisfied and varied between 60.6%and 115.9% both in camellia pollen and cole pollen. Relative standard deviation （R.S.D.%） ranged from 1.2% to 13.1%. Sample analysis indicated water lily pollen is deeply affected by sediment polluted severely.