Simultaneous determination of blockers and agonists by on-fiber derivatization in self-made solid-phase microextraction coating fiber.
Simultaneous determination of blockers and agonists by on-fiber derivatization in self-made solid-phase microextraction coating fiber.
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DOI：
10.1016/j.talanta.2014.07.064
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发表时间：
2015-01
期刊：
影响因子：
6.1
通讯作者：
W. Liu;Zhiming Yan;Xiayang Huang;Jinfeng Chen;Minghua Lu;Lan Zhang;Guonan Chen
中科院分区：
文献类型：
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作者：
W. Liu;Zhiming Yan;Xiayang Huang;Jinfeng Chen;Minghua Lu;Lan Zhang;Guonan Chen
建立了一种环境友好、灵敏度高的测定受体阻滞剂和受体激动剂的方法。该方法是基于自制的溶胶-凝胶固相微萃取（SPME）涂层，同时对纤维衍生化和随后的气相色谱质谱（GC/MS）分析。考察了自制纤维涂层的种类、厚度、衍生化条件、萃取条件和解吸条件等主要因素对固相微萃取的影响。该方法的检测限低于0.2 ng mL−1。克仑特罗在0.5-150 ng mL− 1范围内呈线性，美托洛尔和普萘洛尔在1.0-100 ng mL− 1范围内呈线性。测量值的变化（重复性）低于8.7%（n=6），差异程度（再现性）低于11.4%（n=3）。在应用中，对加标的人唾液样品和真实的人唾液样品进行了分析，发现当普萘洛尔含量很低时，唾液会影响普萘洛尔的检测。所建立的方法在实际应用中是可行的，有助于竞争中激动剂和阻断剂的初步筛选。
An environmentally friendly and sensitive method for determination of blockers and agonists was described in this paper. The method is based on a homemade sol–gel solid-phase microextraction (SPME) coating with simultaneous on-fiber derivatization and subsequent gas chromatography mass spectrometry (GC/MS) analysis. The influences of the main factors on the type and thickness of the homemade fiber coatings, conditions of the derivatization, extraction and desorption of SPME were investigated in detail. The proposed procedure showed limits of detection lower than 0.2 ng mL−1. The linearity was in the 0.5–150 ng mL−1for clenbuterol and 1.0–100 ng mL−1for metoprolol and propranolol. The variation in measurements (repeatability) was below 8.7% (n=6) and the degree of difference between (reproducibility) was below 11.4% (n=3). In the application, spiked human saliva samples and real human saliva samples were analyzed, it was found that saliva would affect the detection of propranolol when it was a very low content. The established method can be feasible in practical application and helpful for agonists and blockers preliminary screening during the competition.