毛细管带电泳法测定饮料和尿液样品中的钾含量

Jatinder Singh Aulakh, Agnes Fekete, Ashok Kumar Malik, Ph. Schmitt-Kopplin, R.K Mahajan
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引用次数: 2

摘要

采用Megabond Elut C18和Strata X 33 μm聚合物吸附剂进行固相萃取预富集,建立了毛细管区带电泳(CZE)二极管阵列检测器(DAD)同时测定百草灭(PQ)和双喹酮(DQ)的条件。以pH、pH(3.8)乙酸钠缓冲液中EDTA的浓度为基准,以3- 8%的甲醇、乙醇和乙腈为背景电解质有机改性剂,对工艺条件进行优化。采用可变波长紫外检测法测定每种化合物的最大吸收,灵敏度高。这些化合物从不同浓度的水样中回收率超过90%。检测限(S/N=3)得到的毫q水加标后,DQ为0.17 ppm, PQ为0.19 ppm,自来水样品中DQ为0.27 ppm, PQ为0.31 ppm,可乐饮料中DQ为0.29 ppm, PQ为0.35 ppm,尿液样品中diquat为0.36 ppm, PQ为0.41 ppm,未预浓缩。使用聚合物滤筒进行预浓缩后,dq的检出限降至2.5 ppb, PQ的检出限降至3 ppb。这些检测限允许在美国环境保护局规定的水平上对这些化合物进行分析。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
Determination of Quats in Beverages and Urine Samples by Capillary Zone Eletrophoresis

Conditions have been developed for simultaneous determination of paraquat (PQ) and diquat (DQ) by capillary zone electrophoresis (CZE) with diode array detector (DAD) after their preconcentration by solid phase extraction using Megabond Elut C18 and Strata X 33 μm Polymeric sorbent cartridges. Conditions were optimised with reference to pH, EDTA concentration in sodium acetate acetic acid buffer of pH (3.8) with 3-8 % of methanol, ethanol and acetonitrile as organic modifier in the background electrolyte. UV detection with variable wavelength was used to determine each compound at its maximum absorption providing an excellent sensitivity. The recovery of these compounds from water samples spiked at different levels was more than 90 %. The limit of detection (S/N=3) obtained for milli-Q water when spiked with standards was 0.17 ppm for DQ and 0.19 ppm for PQ, in tap water samples it was found to be 0.27 ppm for DQ and 0.31 ppm for PQ, in cola beverages it was found to be 0.29 ppm for DQ and 0.35 ppm for PQ, and for the urine samples it was 0.36 ppm for diquat and 0.41 ppm for the PQ without preconcentration. After preconcentration using polymeric cartridge the detection limit was reduced to 2.5 ppb for DQand 3 ppb for PQ for the milli-Q water. These detection limits allows for the analysis of these compounds at the levels established by the US Environmental Protection agency.

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