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超高效液相色谱-串联质谱法直接进样测定水样中8种有机污染物

Determination of 8 Organic Pollutants in Drinking Waters by Ultra-high Performance Liquid Chromatography Tandem Mass Spectrometry with Direct Injection

  • 摘要: 2011年我国实施了新的生活饮用水卫生标准,卫生指标扩展至106项,并配套了相关的检测方法,其中微囊藻毒素、莠去津采用液相色谱紫外检测器的检测方法;丙烯酰胺、灭草松、2,4-D采用气相色谱-电子捕获检测器的检测方法;呋喃丹、草甘膦采用液相色谱荧光检测器的检测方法。这些检测方法均有前处理程序繁琐、工作量大、可操作性差的缺点,在实际工作中应用较为困难。本文采用超高效液相色谱-串联质谱技术(UPLC-MS/MS),建立了水样过0.22 μm滤膜,直接进样测定自来水、地下水及地表水中8种有机污染物(草甘膦、呋喃丹、灭草松、莠去津、2, 4-滴、丙烯酰胺、微囊藻毒素-RR和微囊藻毒素-LR)的分析方法。8种化合物在各自的线性范围内线性关系良好,相关系数均不低于0.993,定量下限为0.07~5 μg/L,低、中、高三个加标水平的回收率为94.2%~103.7%,相对标准偏差为1.1%~7.8%。本文建立的方法操作简便,可以实现在6 min内一次性分析8种目标化合物,与国家标准方法相比,显著提高了分析效率;与文献报道的均是单一类化合物检测方法相比,本检测方法具有相似的灵敏度和检测限,但是目标化合物覆盖更全面,分析时间更短。

     

    Abstract: In 2011, new healthy standards for drinking water were implemented, which included 106 health indicators and related detection methods. In the national standard methods, microcystins and atrazine are detected by Liquid Chromatography with Ultraviolet Detector; acrylamide, bentazone and 2,4-D are detected by Gas Chromatography with Electron Capture Detector, carbofuran and glyphosate are measured by Liquid Chromatography with Fluorescence Detector. All of these methods are cumbersome and have poor operability making them difficult to conduct on a daily basis. A method for the analysis of 8 organic pollutants (glyphosate, carbofuran, bentazone, atrazine, 2,4-D, acrylamide, microcystin-RR and microcystin-LR) in drinking water, surface water and underground water was developed using Ultra Performance Liquid Chromatography with Tandem Mass Spectrometry (UPLC-MS-MS). After filtration by 0.22 μm membrane, the water sample was injection directly into the equipment. Compared with recently reported methods, similar precision and accuracy were obtained and are presented in this paper. But shorter analysis time is needed and more target compounds are included. The result indicate that the LOQ of 8 compounds ranged from 0.07 to 5 μg/L, Meanwhile, the high correlation coefficients (r>0.993) of 8 compounds were obtained within the respective linear ranges. The average recoveries at low, intermediate and high spiked levels range from 96.7% to 101.7% with relative standard deviations (RSD, n=6) of 1.1%-3.5%. This method is suitable for the identification and quantification of the aforementioned 8 compounds in drinking water with the advantages of simple pretreatment, good reliability and high sensitivity.

     

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