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作 者:叶曦雯[1] 牛增元[1] 姚鹏[2] 王卉卉[1,3] 罗忻[1] 许辉[1]
机构地区:[1]山东出入境检验检疫局,山东青岛266002 [2]中国海洋大学化学化工学院,山东青岛266100 [3]青岛科技大学环境与安全工程学院,山东青岛266042
出 处:《分析测试学报》2010年第5期449-454,共6页Journal of Instrumental Analysis
基 金:2007年国家质检公益性行业科研专项基金资助项目(10-66)
摘 要:建立了木材及木制品中10种有机氯杀虫剂残留的气相色谱测定方法。样品经粉碎后,用丙酮-正己烷(体积比1∶9)超声提取20 min,以3 000 r/min离心5 min,重复提取1次,上清液经浓缩、脱水后供气相色谱测定。采用HP-5毛细管气相色谱柱进行分离,ECD检测器进行检测。方法在5-500μg/L的范围内线性关系良好,除4,4′-DDT外,线性相关系数均大于0.995。10种有机氯杀虫剂在松木及密度板空白基质中的加标回收率为89%-110%,相对标准偏差小于8.9%。该方法检出1种白橡木实木样品中含有γ-HCH,含量平均值为0.850 mg/kg,相对标准偏差为1.9%;1种复合木地板样品中含有氯丹杀虫剂,含量平均值为109.134 mg/kg,相对标准偏差为4.7%。该方法操作简单、高效,且灵敏度高、精密度好。A gas chromatographic(GC) method was established for the simultaneous determination of 10 organochlorine pesticides in wood preservatives and treated timber.After being crushed,the wood samples was supersonic extracted with acetone-hexane(1∶9,by volume) for 20 min,followed with centrifugal treatment at the speed of 3 000 r/min for 5 min.The supernatant was evaporated to nearly dry under a gentle stream of nitrogen(N2) and redissolved with hexane.After removing water with anhydrous sodium sulfate(Na2SO4),the solution was determined by GC with electron capture detector(ECD).The method showed a good linearity in the range of 5-500 μg/L,and the correlation coefficients were all above 0.995 except for 4,4′-DDT.The average recoveries of 10 organochlorine pesticides at three spiked concentration levels ranged from 89% to 110%,with RSDs less than 8.9%.This method was also used in the samples.It was found that an oak wood contained γ-HCH pesticide and the average content was 0.850 mg/kg with RSD of 1.9%.Another positive sample was a kind of floor board contained chlordane,and the average content was 109.134 mg/kg,with RSD of 4.7%.This method was simple,sensitive and effective.
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