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A fast and low-cost method for determination of melamine in soil and sediment using high performance liquid chromatography

机译:一种快速和低成本的方法,用于使用高效液相色谱法测定土壤和沉积物中的三聚氰胺

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This paper describes a fast and low-cost method for determination of melamine, an emerging environmental contaminant, in soil and sediment using ultrasonic-assisted extraction coupled with high performance liquid chromatography. The parameters used for sample pretreatment and chromatographic analysis were tested and optimized. The samples were extracted by 5% (v/v) ammonia in methanol with ultrasonic assistance for 5 min, followed by centrifugation and nitrogen blowing, without a cleaning procedure such as solid phase extraction. Chromatographic separation was achieved by a cyano column using acetonitrile/water (5/95, v/v) as the mobile phase containing no ion-pair reagent, and the quantification was carried out by an external standard method. An excellent linearity for melamine was obtained over the concentration range of 0.05a€“5 mg kga?’1 with a correlation coefficient of 0.9999. The limit of detection (S/N = 3) and the limit of quantification (S/N = 10) for melamine were 0.01 mg kga?’1 and 0.04 mg kga?’1, respectively. The recovery for melamine ranged from 95.0% to 105.9%, with relative standard deviations (RSDs) (n = 3) of 1.6a€“5.3%. The proposed method was shown to be simple, rapid, cheap, sensitive and accurate, and was applied to the analysis of melamine in soil and sediment samples with satisfactory results.
机译:本文介绍了使用超声波辅助萃取与高效液相色谱相结合的超声波辅助提取来测定三聚氰胺,新出现的环境污染物,土壤和沉积物的快速和低成本方法。测试和优化用于样品预处理和色谱分析的参数。将样品用5%(v​​ / v)氨在甲醇中提取5%(V / v)氨,超声辅助5分钟,然后离心和氮气吹,无需清洁过程,例如固相萃取。使用乙腈/水(5/95,v / v)作为含有离子对试剂的流动相的乙腈/水(5/95,v / v)实现色谱分离,通过外标方法进行定量。在0.05A€“5mg kga kga'1的浓度范围内获得了三聚氰胺的优异线性度,其相关系数为0.9999。三聚氰胺的检测极限(S / N = 3)和三聚氰胺的定量极限分别为0.01mg kgaα1和0.04mg kga'1。三聚氰胺的回收率范围为95.0%至105.9%,相对标准偏差(RSD)(N = 3)为1.6A€“5.3%。该方法显示出简单,快速,廉价,敏感和准确,并应用于土壤和沉积物样品中三聚氰胺的分析,结果令人满意。

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