Kuo T L
Forensic Sci Int. 1987 Mar;33(3):177-85. doi: 10.1016/0379-0738(87)90126-5.
Homogenized tissue was deproteinized with sulfuric acid. Paraquat in the supernatant was quantificated directly with the dithionite reagent (step 1) or concentrated by the XAD-2 column chromatographic technique before paraquat determination (step 2). Tissue paraquat levels in the range of 0.01-75 mg/kg could be quantificated by second-derivative or zero-order spectroscopy using 2.5 g of tissues. The sensitivity could be increased tenfold by using 25 g of tissue samples. The coefficients of variation of within-run and day-to-day precisions of spiked paraquat in tissue homogenates were below 5% at concentrations of 10.0, 1.0 and 0.1 mg/kg, respectively. The recoveries of the spiked paraquat in tissues ranging from 0.1-10 mg/kg were 91% by step 1 and 74% by step 2. Using these simple methods, steps 1 and 2, the paraquat concentrations in the psoas muscle, liver, lung and kidneys of a swine dosed with 0.16 g/kg of paraquat were investigated. The results were in close agreement with those of the TCA deproteinization method followed by cation-resin column chromatography. The proposed method offers the advantages of simplicity, rapidity, reasonable sensitivity and a wide range of concentrations.
将匀浆组织用硫酸进行脱蛋白处理。上清液中的百草枯可直接用连二亚硫酸盐试剂进行定量(步骤1),或者在测定百草枯之前通过XAD - 2柱色谱技术进行浓缩(步骤2)。使用2.5克组织,通过二阶导数或零阶光谱法可对0.01 - 75毫克/千克范围内的组织百草枯水平进行定量。使用25克组织样本可使灵敏度提高10倍。在组织匀浆中添加百草枯,浓度分别为10.0、1.0和0.1毫克/千克时,批内和日间精密度的变异系数均低于5%。在组织中添加0.1 - 10毫克/千克的百草枯,步骤1的回收率为91%,步骤2的回收率为74%。使用这两种简单方法(步骤1和步骤2),对用0.16克/千克百草枯给药的猪的腰大肌、肝脏、肺和肾脏中的百草枯浓度进行了研究。结果与采用三氯乙酸脱蛋白法继以阳离子树脂柱色谱法得到的结果非常一致。所提出的方法具有简单、快速、灵敏度合理以及浓度范围宽等优点。