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衍生化固相微萃取-色谱质谱法快速检测猪尿中的β-受体兴奋剂
Quick Analysis of β-Agonists in Urine by Solid Phase Microextractionwith Headspace Derivatization and Gas Chromatography-Mass Spectrometry
【摘要】 应用固相微萃取法提取猪尿中的盐酸克仑特罗 ,经顶空衍生后以GC MS法测定。聚丙烯酸酯纤维对克仑特罗吸附良好 ,萃取温度、时间、溶液的pH值 ,以及衍生温度、时间、衍生剂用量等影响因素经过优化。方法线性范围为 1~ 5 0 0 μg L ,检出限为 0 .5 μg L。方法快速、灵敏 ,其相对标准偏差为 3 .9%~ 6.8% ,标准加入回收率为 82 .0 %~ 87.7%。
【Abstract】 Clenbuterol in urine was extracted by solid-phase microextraction, and headspace derivatized by N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA), then analyzed by selected ion monitor of gas chromatography-mass specdtrometry (GC-MS). An 85 μm polyacrylate fiber can adsorb clenbuterol well. Extraction and derivatization conditions such as extraction time, temperature, pH, derivatization time, temperature, and the amount of derivatizing reagent have been optimized. The linear range for the analysis is 1~500 μg/L, with detection limits of 0.5 μg/L. The method has the advantages of quick operation and high sensitivity with the recovery of 82.0%~87 7% and relative standard deviation of 3 9%~6.8%.
【Key words】 Solid phase microextraction; clenbuterol; headspace derivatization; gas chromatography-mass spectrometry;
- 【文献出处】 分析化学 ,Chinese Journal of Analytical Chemistry , 编辑部邮箱 ,2003年03期
- 【分类号】O657.63
- 【被引频次】18
- 【下载频次】165