DETERMINATION OF SELECTED ORGANOCHLORINE PESTICIDES AND POLYCHLORINATED-BIPHENYLS IN HUMAN SERUM

DETERMINATION OF SELECTED ORGANOCHLORINE PESTICIDES AND POLYCHLORINATED-BIPHENYLS IN HUMAN SERUM
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DOI:
10.1093/jat/14.3.137
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发表时间:
1990-05-01
影响因子:
2.5
通讯作者:
NEEDHAM, LL
NEEDHAM, LL
中科院分区:
医学3区
文献类型:
--
作者:
BURSE, VW;HEAD, SL;NEEDHAM, LL

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本文介绍了一种测定血清中某些氯代农药和多氯联苯(如多氯联苯1260)残留量的方法。该方法包括以下步骤:(1)用有机溶剂提取变性血清;(2)通过微弗罗里硅土柱洗脱有机提取物,获得两个级分;(3)对极性较低的弗罗里硅土级分进行酸处理,随后通过失活硅胶洗脱,获得两个级分;(4)使用气液色谱法和电子捕获检测器分析所有三个级分。该方法产生的10种农药在1-10.7 ppb的范围内的50.4%至121.6%的体外加标回收率,在4.98-21 ppb的范围内,回收率范围为47.7至112.6。Aroclor 1260的体内“回收率”平均为104.8%,浓度水平为约100 mg/L时为92.3%。10和. apprx。30 ppb。该方法不能与更常用的己烷提取技术进行比较,因为这些提取物对气相色谱系统具有有害影响。
A method is presented that can be used to determine the residue level of certain chlorinated pesticides and polychlorinated biphenyls (as Aroclor 1260) in serum. The method involves the following: (1) extraction of denatured serum with organic solvents; (2) elution of the organic extract through micro-Florisil columns to obtain two fractions; (3) acid treatment of the less polar Florisil fraction and its subsequent elution through deactivated silica gel to obtain two fractions; and (4) analysis of all three fractions using gas-liquid chromatography with electron capture detection. The method produced in vitro recoveries for 10 pesticides spiked in the range of 1-10.7 ppb of 50.4% to 121.6%, and in the range of 4.98-21 ppb, recoveries ranged from 47.7 to 112.6. In vivo "recoveries" of Aroclor 1260 averaged 104.8% and 92.3% for concentration levels of .apprx. 10 and .apprx. 30 ppb, respectively. The method could not be compared with the more commonly used hexane extraction technique because of the deleterious effect these extracts had on the gas chromatographic system.