测定灭鼠剂中抗凝血剂的新通用方法

S. Andreev, E. S. Belyaev, A. Ischenko
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引用次数: 1

摘要

固体石蜡块是一种最先进的杀鼠诱饵,因为它可以保护它免受环境暴露,并且不会降低啮齿动物的适口性。本文提出了一种简便、通用的测定固体型煤中溴二酮、溴二酮和异芬酮含量的方法。固体型煤是由石蜡、毒物和填充物混合而成,可用于粮食、面粉等。分析含石蜡鱼饵的难点在于如何去除它。为此,我们建议在体系中采用己烷-乙腈萃取。石蜡可溶于己烷,而溴二酮、溴二酮和异二酮不能溶于己烷。用分离漏斗对所得两相体系进行分离,并收集底部馏分。如果样品中存在任何填充物,则将其过滤,直到混合物被分离,残留物用乙腈洗涤。在将样品引入色谱仪之前,用孔隙率为0.45µm的PTFE过滤器过滤两次。采用Thermo Acclaim®表面活性剂色谱柱,以乙腈和0.1 M醋酸铵水溶液(pH 5.4)为流动相,梯度洗脱,达到最佳分离效果。所有三种毒物都在264 nm的波长检测到。该方法灵敏度为0.028 mg。线性范围为0.00067 ~ 0.01%。溴代隆的回收率为94%,溴代醌的回收率为98%,异芬醌的回收率为90%。
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NEW UNIVERSAL METHOD FOR DETERMINATION OF ANTICOAGULANTS IN RODENTICIDES
Solid paraffin briquettes are one of the most modern types of rodenticide baits, because they protect it from the environmental exposure and do not reduce palatability of rodents. This paper proposes a simple universal method for the determination of brodifacoum, bromadiolone and difenacoum in solid briquettes, which are a mixture of paraffin, poison and filler, which can be used as grain, flour and the like. The difficulty in the analysis of baits containing paraffin, is to get rid of it. For this, we propose to use hexane-acetonitrile extraction in the system. Paraffin dissolves in hexane, while brodifacoum, bromadiolone and difenacoum do not. The resulting two-phase system was separated using a separatory funnel and the bottom fraction was collected. If any fillers were present in the sample, they were filtered until the mixture was separated, the residue was washed with acetonitrile. Before introducing the sample into the chromatograph, it was filtered twice with PTFE filters with a porosity of 0.45 µm. The best separation was achieved using a Thermo Acclaim® Surfactant column using acetonitrile and 0.1 M aqueous ammonium acetate solution (pH 5.4) as the mobile phase in a gradient elution mode. All three poisons were detected at a wavelength of 264 nm. This method has a sensitivity of 0.028 mg. The linearity range is from 0.00067 to 0.01%. The recovery rate for bromadiolone is 94%, for brodifacoum, 98%, and for difenacoum, 90%.
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