花粉中有机氯类农药串联固相萃取柱净化——气相色谱分析  

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

作　　者：陈芳[1] 薛晓锋[1] 赵静[1] 

机构地区：[1]中国农科院蜜蜂研究所,农业部蜂产品质量监督检验测试中心(北京),北京100093

出　　处：《中国蜂业》2009年第2期5-8,共4页Apiculture of China

基　　金："十一五"国家科技支撑项目-蜂产品高效利用与安全生产技术(2006BAD06B04)

摘　　要：本文旨在研究应用气相色谱—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2.64～6.62。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。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.

关 键 词：有机氯农药 蜂花粉 固相萃取 气相色谱 

分 类 号：S896.4[农业科学—特种经济动物饲养]