【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7 cm的聚丙烯中空纤维,在样品溶液pH11、磁力搅拌速度1 000 r/min、室温条件下萃取20 min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30~6 000μg/kg之间,线性相关系数(r2)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。更多还原

【Abstract】 Objective: A novel hollow fiber-based liquid phase microextraction(HF-LPME) coupled with high performance 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 15 μL 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 30~6 000 μg/kg of the compound in pork with the correlation coefficient(r2) of 0.9995 and the detection limit of 2.4 μg/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.更多还原