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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:高效液相色谱法快速,低成本地测定土壤和沉积物中的三聚氰胺

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摘要

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 0.05-5 mg kg~(-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 kg~(-1) and 0.04 mg kg~(-1), respectively. The recovery for melamine ranged from 95.0% to 105.9%, with relative standard deviations (RSDs) {n = 3) of 1.6-5.3%. 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:本文介绍了一种超声波辅助萃取与高效液相色谱法测定土壤和沉积物中三聚氰胺(一种新兴的环境污染物)的快速,低成本方法。测试和优化了用于样品预处理和色谱分析的参数。样品在超声辅助下用5%(v​​ / v)的甲醇氨溶液萃取5分钟,然后离心和吹氮气,无需进行诸如固相萃取的清洁程序。通过氰基色谱柱分离色谱,使用不含离子对试剂的乙腈/水(5/95,v / v)作为流动相,并通过外标法进行定量。在0.05-5 mg kg〜(-1)的浓度范围内,三聚氰胺具有良好的线性,相关系数为0.9999。三聚氰胺的检出限(S / N = 3)和定量限[S / N = 10)分别为0.01 mg kg〜(-1)和0.04 mg kg〜(-1)。三聚氰胺的回收率为95.0%至105.9%,相对标准偏差(RSD){n = 3)为1.6-5.3%。结果表明,该方法简便,快速,廉价,灵敏,准确,可用于土壤和沉积物中三聚氰胺的分析,结果令人满意。

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