中空纤维液相微萃取-高效液相色谱法测定猪肉中盐酸克伦特罗残留  

Determination of Clenbuterol in Pork by Hollow Fiber-based Liquid Phase Microextraction Coupled with High Performance Liquid Chromatography

作　　者：刘志梅[1] 陈永艳[1] 杨秀敏[1] 王春[1] 刘伟华[1] 王志[1] 

机构地区：[1]河北农业大学理学院生物无机重点实验室,河北保定071001

出　　处：《中国食品学报》2009年第2期171-175,共5页Journal of Chinese Institute Of Food Science and Technology

基　　金：河北省自然科学基金资助项目(B2006000413)

摘　　要：目的：基于中空纤维的液相微萃取（HF—LPME）新技术，建立猪肉组织中盐酸克伦特罗的液相色谱分析方法。方法：采用中空纤维液相微萃取和液相色谱联用技术，对影响HF—LPME的试验条件进行优化。经过优化，选用7cm的聚丙烯中空纤维．在样品溶液pH11、磁力搅拌速度1000r／min、室温条件下萃取20min后，将有机溶剂在氮气流下吹干，用15μL甲醇溶解，进样10μL，做色谱分析。结果：在优化的试验条件下，克伦特罗的富集倍数为78倍，线性范围在30-6000μg／kg之间，线性相关系数（r^2）0．9995，检出限2．4μg／kg（S／N=3）。将该方法用于猪肉组织中克伦特罗的测定，低、中、高3种浓度的加标回收率分别为84．9％、91．4％和95．0％，相对标准偏差（RSD）分别为6．3％、5．8％和4．6％。结论：该方法操作简便、环境友好，具有较高的灵敏度．适于猪肉中盐酸克伦特罗残留的检测。Objective： A novel hollow fiber-based liquid phase microextraction （HF-LPME） coupled with high performauee liquid chromatography （HPLC） for the determination of clenbuterol in pork was developed. Methods： Some important extraction parameters, such as the effect of the pH of the sample solution, extraction time, stirring rate and salt concentration were optimized. On the basis of the experiments, the optimal HF-LPME conditions were selected as follows： the pH of sample solution（donor phase） was 11. Toluene was used as extraction solvent. The extractions were conducted for 20 min at a stirring rate of 1 000 r/min. After extraction, the extraction solvent was evaporated to dryness under a stream of nitrogen at room temperature. The residue was dissolved in 15μL methanol, and then a volume of 10 μL was injected onto the HPLC system for analysis. Results： The new method provided a good average enrichment times of 78 for clenbuterol. A good linear relationship existed in the range of 30-6 000μg/kg of the compound in pork with the correlation coefficient （r^2） of 0.9995 and the detection limit of 2.4μg/kg（S/N=3：1）. The recoveries at three concentration levels were 84.9%, 91.4% and 95.0%, respectively, with the relative standard deviations ranging from 4.6% to 6.3%. Conclusion： The method was shown to be simple, sensitive and environment-friendly, and was suitable for the determination of residual clenbuterol in pork.

关 键 词：中空纤维液相微萃取 高效液相色谱 盐酸克伦特罗 猪肉 

分 类 号：S859.84[农业科学—临床兽医学]