DETERMINATION OF THE HERBICIDES PARAQUAT AND DIQUAT IN BLOOD AND URINE BY GAS-CHROMATOGRAPHY
DETERMINATION OF THE HERBICIDES PARAQUAT AND DIQUAT IN BLOOD AND URINE BY GAS-CHROMATOGRAPHY
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DOI：
10.1016/s0021-9673(00)96258-7
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发表时间：
1984-01-01
期刊：
影响因子：
--
通讯作者：
UKAI, S
中科院分区：
文献类型：
--
作者：
KAWASE, S;KANNO, S;UKAI, S
描述了一种气相色谱方法，用于测定人血液和尿液中的百草枯 (1) 和敌草快 (2)，其中 1 或 2 通过添加 Reinecke 试剂很容易沉淀为其 Reeckate 复合物（3 和 4），尽管血液需要用 3.4% 高氯酸或 10% 三氯乙酸进行脱蛋白。沉淀在室温下1小时内完成，3和4通过用硼氢化钠和氯化镍(II)的混合物处理很容易还原，得到来自4的相应全氢化产物1,1''-二甲基-4,4''-联哌啶(5)和3以及反式-和顺式-全氢二吡啶并[1,2-a:2'',1''-c]吡嗪(6)。全氢化产物通过 GLC 测定，不受血液和尿液原始成分的干扰。 GLC方法（在Chromosorb W AW DMCS上含有5% Apiezon L的5% KOH溶液）适合于用氢火焰离子化检测同时测定血液和尿液中1-70 μg/ml（0.7-50.7 μg/ml作为1离子；0.5-35.6 μg/ml作为2离子）的血液和尿液中的1和2。该方法可适用于死后组织中化学物质和土壤中污染物的测定。
A gas chromatographic method was described for determining paraquat (1) and diquat (2) in human blood and urine where 1 or 2 was readily precipitated as its reineckate complex (3 and 4) by addition of Reinecke reagent, although blood required deproteination with 3.4% perchloric acid or 10% trichloroacetic acid. The precipitation was completed in 1 h at room temperature and 3 and 4 were easily reduced by treatment with a mixture of sodium borohydride and nickel(II) chloride to afford corresponding perhydrogenated products, 1,1''-dimethyl-4,4''-bipiperidine (5) and 3 and trans- and cis-perhydrodipyrido[1,2-a:2'',1''-c] pyrazine (6) from 4. The perhydrogenated products were determined by GLC without interference from the original components of the blood and urine. The GLC method (5% KOH solution with 5% Apiezon L on Chromosorb W AW DMCS) was suitable for simultaneous determination with hydrogen flame-ionization detection in the range 1-70 .mu.g/ml (0.7-50.7 .mu.g/ml as 1 ion; 0.5-35.6 .mu.g/ml as 2 ion) of 1 and 2 in blood and urine. The method could be applicable to the determination of the chemicals in postmortem tissue and as pollutants in soils.