中文核心期刊

中国科技核心期刊

CSCD来源期刊

DOAJ 收录

Scopus 收录

李晓亚, 张莉, 桂建业, 张永涛, 张辰凌, 赵国兴, 田来生. 膜萃取与超声衍生联用-负化学源质谱法测定地下水中酚类化合物[J]. 岩矿测试, 2014, 33(2): 270-274.
引用本文: 李晓亚, 张莉, 桂建业, 张永涛, 张辰凌, 赵国兴, 田来生. 膜萃取与超声衍生联用-负化学源质谱法测定地下水中酚类化合物[J]. 岩矿测试, 2014, 33(2): 270-274.
Xiao-ya LI, Li ZHANG, Jian-ye GUI, Yong-tao ZHANG, Chen-ling ZHANG, Guo-xing ZHAO, Lai-sheng TIAN. Determination of Phenols in Groundwater by Solid-Phase Membrane Extraction Combined with Ultrasonic Derivatization-negative Chemical Ionization Mass Spectrometry[J]. Rock and Mineral Analysis, 2014, 33(2): 270-274.
Citation: Xiao-ya LI, Li ZHANG, Jian-ye GUI, Yong-tao ZHANG, Chen-ling ZHANG, Guo-xing ZHAO, Lai-sheng TIAN. Determination of Phenols in Groundwater by Solid-Phase Membrane Extraction Combined with Ultrasonic Derivatization-negative Chemical Ionization Mass Spectrometry[J]. Rock and Mineral Analysis, 2014, 33(2): 270-274.

膜萃取与超声衍生联用-负化学源质谱法测定地下水中酚类化合物

Determination of Phenols in Groundwater by Solid-Phase Membrane Extraction Combined with Ultrasonic Derivatization-negative Chemical Ionization Mass Spectrometry

  • 摘要: 酚类化合物由于极性较大,无法直接用气相色谱-质谱法测定,需要通过衍生来降低其极性,提高检测灵敏度;但是传统的衍生步骤繁琐,干扰因素多,操作难度大。本文对传统的前处理方法进行改进,建立了固相膜萃取、超声衍生负化学源质谱测定地下水中酚类化合物的方法。水样萃取后将萃取膜直接放入衍生瓶中,利用超声波的作用力将洗脱和衍生合二为一,超声完成后将溶液直接上机进行测定。测定低、中、高三个浓度水平的加标样品,各目标物的回收率均能达到70%~90%,检出限在0.25~0.35 μg/L之间,相对标准偏差小于10%,能够满足地下水中酚类物质的检测要求。本方法将洗脱和衍生集于一体,使用2 mL丙酮进行洗脱和衍生就可将全部目标物回收,简化了操作步骤,减少了有机溶剂的使用量;同时由于洗脱和衍生是在密闭的环境中进行,外界因素引入的干扰少,克服了二次污染的问题,测定数据更加可靠。

     

    Abstract: Due to their strong polarity, phenolic compounds cannot be directly determined by Gas Chromatography-Mass Spectrometry. Derivatization can reduce the strength of the polarity of phenols, and improve the detection sensitivity. However, the traditional derivative steps are tedious, with many interference factors and complex operations. By applying improvements to the traditional pretreatment method, phenols in groundwater were measured through solid-phase membrane extraction combined with Ultrasonic Derivatization-Negative Chemical Ionization Mass Spectrometry. The membrane was transferred into a derivative bottle after extraction, and then the elution and derivatization were processed simultaneously using ultrasound. The solution was determined by Gas Chromatography-Negative Chemical Ionization Mass Spectrometry directly. By determining the spiked samples at different concentration levels, the recoveries of the method for target components are in the range of 70%-90%, the detection limits are 0.25-0.35 μg/L and relative standard deviations (RSD) are less than 10%. The proposed method simplifies the traditional tedious steps by using 2 mL acetone for elution and derivation. All target objectives have good recoveries. Due to conducting the elution and derivation processes in an airtight environment, less interference factors were introduced without the problem of secondary pollution, and consequently the data were more reliable.

     

/

返回文章
返回