动物尿液中盐酸克伦特罗的分子印迹固相萃取-气相色谱-质谱法研究  

Molecularly Imprinted Polymer Solid Phase Extraction Coupled with Gas Chromatography-Mass Spectrometry for the Determination of Trace Clenbuterol Hydrochloric in Animal Urine

作　　者：王培龙[1] 范理[1] 宋荣[1] 高生[1] 苏晓鸥[1] 杨曙明[1] 

机构地区：[1]中国农业科学院农业质量标准与检测技术研究所,北京100081

出　　处：《分析化学》2007年第9期1319-1322,共4页Chinese Journal of Analytical Chemistry

基　　金："948引进国际先进农业科学技术"基金资助项目(No.2003Q0808)

摘　　要：采用分子印迹聚合物（MIP）固相萃取小柱提取、净化并富集猪尿液中的盐酸克伦特罗分子，用N，O-双三甲基硅基三氟乙酰胺（BSTFA）衍生化，毛细管气相色谱-质谱联用（选择离子模式，选择离子为277、262、243和86）对衍生物分析。优化了MIP固相萃取柱的淋洗条件，考察了MIP固相萃取柱的净化效果和消除基体干扰能力，建立了对动物尿液中盐酸克伦特罗的定性、定量分析的方法。在优化条件下，本法检出限（LOD）为0．51μg／L，定量限（LOQ）为1．00μg／L；不同盐酸克伦特罗加入量的回收率为71．0％～89．3％；相对标准偏差为3．2％～9．7％。将该方法与农业行业标准方法比较，结果吻合较好。但该方法灵敏度和精密度高，操作更为简单、快捷。The clenbuterol hydrochloric in animal imprinted polymer （ MIP ） solid phase extraction urine was extracted and concentrated using molecularly cartridge and determined by gas chromatography-mass spectrometry （selected ion mode, the selected ions are： 277, 262, 243 and 86） after derivatization of the purified sample with N, O-his （trimethylsilyl） trifluoroacetamide （BSTFA）. The clean-up procedure was optimized, the clean effect and the matrix effect of the MIP cartridge were examined. A simple qualitative and quantitative analysis method has been developed for the determination of the Clenbuterol hydrochloric in animal urine sample. Under the optimized conditions, the limit of determination is 0.51 μg/L and the limit of quantitative （LOQ） is 1.00μg/L for urine sample, the recoveries of different quantities of clenbuterol hydrochloric are between 71.0% and 89.3 % , the relative standard deviations （RSD） are 3.2% -9.7%. there is a good linear correlation （the calibration coefficient is above 0. 9997） between the ratio of peak areas and the concentration of clenbuterol hydrochloric in the range of 10 - 1000μg/L. The developing method was applied to the determination of clenbuterol hydrochloric in real urine sample, the result is satisfactory comparing to the method of agricultural industrial standards, the precision of the method is high and the manipulation is simple and fast.

关 键 词：分子印迹聚合物 盐酸克伦特罗 气相色谱-质谱 

分 类 号：S859.8[农业科学—临床兽医学]