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首页> 外文期刊>Talanta: The International Journal of Pure and Applied Analytical Chemistry >Blank and sample handling troubleshooting in ultratrace analysis of alkylphenols and bisphenol A by liquid chromatography tandem mass spectrometry
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Blank and sample handling troubleshooting in ultratrace analysis of alkylphenols and bisphenol A by liquid chromatography tandem mass spectrometry

机译:液相色谱串联质谱法对烷基酚和双酚A进行超痕量分析时的空白和样品处理故障排除

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摘要

Blank contamination is a notorious problem in the ultratrace analysis of alkylphenols and bisphenol A. The achievement of low detection limits is complicated due to the high background signals. Furthermore, overestimations and underestimations in the analytical results can occur when blank levels are not stable. Thus, a review of sources of blank contamination in this type of analysis was carried out. Several sources of contamination were identified and useful guidelines are proposed for the determination of these compounds in water samples by liquid chromatography coupled with mass spectrometry. The system contamination was maintained below 0.09 ng (reagent blank) for all compounds and below 0.003 μg L~(-1) (procedure blank). The main improvement was obtained by using LC-MS grade solvent in the mobile phase and PTFE syringe filters for the filtration of the sample extracts. Sample handling aspects such as filtration and storage of the water samples were also considered. The filtration of the samples should be avoided because both contamination and adsorption problems were observed when different kinds of filters were assayed. The refrigerated storage of water samples should be limited to 5 days (without addition of methanol) or 8 days (with 5% methanol).
机译:在烷基酚和双酚A的超痕量分析中,空白污染是一个臭名昭著的问题。由于高背景信号,低检测限的实现非常复杂。此外,当空白水平不稳定时,分析结果中可能会高估和低估。因此,在这种类型的分析中对空白污染物的来源进行了审查。确定了几种污染源,并提出了通过液相色谱-质谱联用法测定水样中这些化合物的有用指南。所有化合物的系统污染均保持在0.09 ng以下(试剂空白),0.003μgL〜(-1)以下(程序空白)。通过在流动相中使用LC-MS级溶剂和PTFE注射器式过滤器对样品提取物进行过滤,可以实现主要的改进。还考虑了样品处理方面,例如水样品的过滤和存储。应避免样品的过滤,因为在分析不同种类的过滤器时会同时观察到污染和吸附问题。水样品的冷藏应限制为5天(不添加甲醇)或8天(5%甲醇)。

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