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首页> 外文期刊>Journal of chromatography, B. Analytical technologies in the biomedical and life sciences >Ultra performance liquid chromatography-tandem mass spectrometry for the determination of amicarthiazol residues in soil and water samples
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Ultra performance liquid chromatography-tandem mass spectrometry for the determination of amicarthiazol residues in soil and water samples

机译:超高效液相色谱-串联质谱法测定土壤和水样中的甲硫唑残留

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摘要

A reliable and rapid method has been optimized to determine the residue of amicarthiazol in soil and environmental water samples. After extraction and evaporation, the extraction was carried out with solid phase extraction (SPE) cleanup using HLB cartridge (only soil samples) and for the quantitative determination by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The resulting residues of amicarthiazol were analyzed by a gradient separation performed on a UPLC system with a C18 column, methanol and water containing 0.1% (v v~(?1)) formic acid as the mobile phase in the mode of electrospray positive ionization (ESI~+) and multiple reaction monitoring (MRM). Results showed that the recoveries for spiked samples were 74.4–97.1% and 72.1–109.9% for soil and water, respectively, with the relative standard deviation (RSD) less than 10.2% when fortified at 10, 100 and 1000 μg L~(?1). The limits of detection (LODs) and the limits of quantification (LOQs) for matrix matched standards ranged from 0.073–0.425 μg L~(?1) and 0.243–1.42 μg L~(?1). The intra-day precision (n = 5) and the inter-day precision over 10 days (n = 10) for the amicarthiazol in soils and water samples spiked at 100 μg L~(?1) was 7.9% and 15.9%, respectively. Results indicated that the developed method could be a helpful tool for the controlling and monitoring of the risks posed by amicarthiazol to human health and environment safety.
机译:优化了一种可靠,快速的方法,可测定土壤和环境水样品中的乙酰胺噻唑残留量。萃取和蒸发后,萃取使用HLB柱(仅土壤样品)进行固相萃取(SPE)净化,并通过超高效液相色谱-串联质谱(UPLC-MS / MS)进行定量测定。通过在UPLC系统上使用C18色谱柱,甲醇和含有0.1%(vv〜(?1))甲酸作为流动相的水以电喷雾正电离(ESI)的方式在UPLC系统上进行梯度分离来分析所得的氨基噻唑残留物〜+)和多反应监测(MRM)。结果表明,加标样品在土壤和水中的回收率分别为74.4–97.1%和72.1–109.9%,在10、100和1000μgL〜(?)下强化时,相对标准偏差(RSD)小于10.2%。 1)。基质匹配标准品的检出限(LOD)和定量限(LOQ)在0.073–0.425μgL〜(?1)和0.243–1.42μgL〜(?1)之间。加标浓度为100μgL〜(?1)的土壤和水样品中的甲硫唑的日内精度(n = 5)和10天之内的日间精度(n = 10)分别为7.9%和15.9% 。结果表明,所开发的方法可能是控制和监测阿米替唑对人体健康和环境安全构成风险的有用工具。

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