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采用热脱附-气相色谱飞行时间质谱法对三甲胺进行准确可靠的分析。

An accurate and reliable analysis of trimethylamine using thermal desorption and gas chromatography-time of flight mass spectrometry.

机构信息

Department of Environment & Energy, Sejong University, Seoul, Republic of Korea.

出版信息

Anal Chim Acta. 2013 May 30;780:46-54. doi: 10.1016/j.aca.2013.03.069. Epub 2013 Apr 16.

Abstract

Trimethylamine (TMA) is well-known for manifesting the odor of rotting fish and urine. The analysis of TMA in environmental samples generally suffers from low reproducibility and poor sensitivity. In this study, a technique for the quantitative analysis of gas phase TMA was developed using thermal desorption (TD)-gas chromatography (GC)-time of flight mass spectrometry (TOF-MS). This new approach yielded good linearity (R(2)=0.9930), precision (RSE=1.59%), and high sensitivity with the method detection limit (MDL) of 51 pg, i.e., detection of 0.021 ppb of TMA at 1L sample (limit of detection (LOD): 5.32 pg (0.002 ppb). This method was tested against gas samples collected from two representative sources of TMA: (1) rotten thornback fish and (2) cat urine-soaked clay. The concentration of TMA in these samples, when analyzed after treatment at varying dilution ratios, averaged 293±29.7 ppm (RSE=3.82%) and 74.1±5.78 ppb (RSE=3.19%), respectively. The feasibility of this approach, when tested with TD-GC-Quadruple (Q) MS, showed a good compatibility with moderately reduced sensitivity. The results of this study demonstrated that one can achieve highly reliable and reproducible analysis of TMA from environmental samples when using thermal desorption (for pretreatment) and detection (by the TOF or Q-MS system).

摘要

三甲胺(TMA)因其具有腐鱼和尿液的气味而广为人知。在环境样品中分析 TMA 通常存在重现性差和灵敏度低的问题。在这项研究中,开发了一种使用热解吸(TD)-气相色谱(GC)-飞行时间质谱(TOF-MS)定量分析气相 TMA 的技术。这种新方法具有良好的线性(R²=0.9930)、精密度(RSE=1.59%)和高灵敏度,方法检测限(MDL)为 51 pg,即 1L 样品中 TMA 的检测限为 0.021 ppb(检测限(LOD):5.32 pg(0.002 ppb)。该方法用于检测两种代表性 TMA 来源的气体样品:(1)腐臭的多宝鱼和(2)猫尿浸湿的粘土。这些样品在经过不同稀释比处理后进行分析,TMA 的浓度分别平均为 293±29.7 ppm(RSE=3.82%)和 74.1±5.78 ppb(RSE=3.19%)。当使用 TD-GC-四极(Q)MS 进行测试时,该方法的可行性显示出与适度降低的灵敏度很好的兼容性。这项研究的结果表明,当使用热解吸(用于预处理)和检测(通过 TOF 或 Q-MS 系统)时,可以对环境样品中的 TMA 进行高度可靠和可重复的分析。

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