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Conversion of a commercial gas chromatography-mass spectrometer to a liquid chromatography -particle beam/glow discharge mass spectrometer

机译:将商用气相色谱-质谱仪转换为液相色谱-粒子束/辉光放电质谱仪

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摘要

Presented here is the evaluation of working parameters necessary to convert a commercially available HP 5973 MSD gas chromatography electron impact mass spectrometer into a liquid chromatography particle beam glow discharge mass spectrometer (LC-PB/GDMS) system. The initial GC unit was replaced with a commercially available PB interface that allows analysis of liquid samples via electron ionization (EI) mass spectrometry. The original EI source has been removed and replaced with a simple, home-built glow discharge (GD) source, allowing both molecular and elemental information to be obtained simultaneously. Nebulization characteristics were optimized with respect to liquid flow, nebulizer gas, desolvation temperature, and the ability to remove solvent by a two-stage momentum separator. Glow discharge source block temperatures and plasma conditions were optimized relative to the caffeine (test compound) responses. The optimized conditions determined in this study are comparable to work done on a similar type of GDMS in this laboratory. Comparisons of analyte responses for the EI and GD sources with the PB interface reveal caffeine detection limits of 34 and 15 ng ML~(-1), respectively. The GD and EI mass spectra for caffeine are similar to those of prior work and the NIST mass spectral library. Analytical responses of 100 μL injections varied from 4.7-9.2% RSDs for concentrations of 0.001-250 μg ML~(-1) of caffeine, creatinine, a tetra-peptide, selenium-methyl-selenocysteine, and Cs and Pb salts. Detection limits were found to be in the ng ML~(-1) level with absolute masses ranging from 0.24-31.4 ng.
机译:这里介绍的是对将商用HP 5973 MSD气相色谱电子冲击质谱仪转换为液相色谱粒子束辉光放电质谱仪(LC-PB / GDMS)系统所需的工作参数的评估。最初的GC单元被市售的PB接口代替,该接口允许通过电子电离(EI)质谱分析液体样品。原始的EI源已被删除,并替换为简单的自制辉光放电(GD)源,从而可以同时获得分子和元素信息。雾化特性针对液体流量,雾化气,去溶剂化温度以及通过两级动量分离器去除溶剂的能力进行了优化。相对于咖啡因(测试化合物)响应,优化了辉光放电源的温度和血浆条件。在这项研究中确定的优化条件与在该实验室中对类似类型的GDMS所做的工作相当。通过PB接口对EI和GD来源的分析物响应进行比较,发现咖啡因的检出限分别为34和15 ng ML〜(-1)。咖啡因的GD和EI质谱与以前的工作和NIST质谱库相似。对于浓度为0.001-250μgML〜(-1)的咖啡因,肌酐,四肽,硒代甲基硒代半胱氨酸以及Cs和Pb盐,100μL进样的分析响应范围为4.7-9.2%RSD。检出限为ng ML〜(-1),绝对质量为0.24-31.4 ng。

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  • 来源
    《Journal of Analytical Atomic Spectrometry》 |2010年第11期|p.1780-1786|共7页
  • 作者单位

    Department of Chemistry, Biosystems Research Complex, Clemson University, Clemson, South Carolina, 29634-0973, USA;

    rnDepartment of Chemistry, Biosystems Research Complex, Clemson University, Clemson, South Carolina, 29634-0973, USA CSS Analytical Co. Inc., 6728 Warwick Ave, Shawnee, KS, 66218, USA;

    rnDepartment of Chemistry, Biosystems Research Complex, Clemson University, Clemson, South Carolina, 29634-0973, USA;

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