中空纤维液相微萃取-高效液相色谱法测定牛奶中3种大环内酯类抗生素残留  

Determination of Three Macrolide Antibiotics in Milk 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] 张美月[1] 宋双居[1] 王春[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1期183-189,共7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：应用基于中空纤维的液相微萃取（HF—LPME）新技术建立牛奶样品中替米考星、麦迪霉素和交沙霉素3种大环内酯类抗生素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的试验奈件进行优化。经过优化．选用7cm的聚丙烯中空纤维，在样品溶液pH8．5、磁力搅拌速度1000r／min及室温条件下萃取20min，在氮气流下吹干有机溶剂，然后用12μL乙腈溶解，进样10μL进行色谱分析。结果：在优化的试验条件下．替米考星、麦迪霉素和交沙霉素的富集倍数分别为34、52和47倍，线性范围均在0．05～5μg／mL之间，相关系数（r^2）分别为0．9978、0．9986和0．9989，检出限分别为5、2和2ng／mL（S/N=3）。该方法用于牛奶中替米考星、麦迪霉素和交沙霉素3种抗生素的测定，加标回收率为79．0％-105.3％，相对标准偏差（RSD）为5．3％．9.4％。结论：该方法操作简便，具有较高的灵敏度，适于牛奶中抗生素残留的检测。Objective： A novel hollow fiber-based liquid phase microextraction （HF-LPME） coupled with high performance liquid chromatography （HPLC） was developed for the determination of three macrolide antibiotics in milk. 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. As a result, the optimal HF-LPME conditions were selected as follows： the pH of sample solution （donor phase） was 8.5 and toluene was used as the extraction solvent. The extractions were conducted for 20 min at a stirring rate of 1 000 r/min. ness under a stream of nitrogen at room temperature. The After extraction, the extraction solvent was evaporated to dryresidue was reconstituted in 12 μL acetonitrile, and then a volume of 10μL was taken to be injected into the HPLC system for analysis. Results： The new method provided good average enrichment times of 34, 52 and 47 for tilmicosin, midecamycin and josamycin, respectively. A good linear relationship existed in the range of 0.05-5μg/mL of each compound in milk with the correlation coefficients （r^2） of 0.9978, 0.9986 and 0.9989 and the detection limits of 5, 2 and 2 ng/mL （S/N=3：1） for tilmicosin, midecamycin and josamycin, respectively. The recoveries were between 79.0% and 105.3% with the relative standard deviations ranging from 5.3% to 9.4%. Conclusion： The method was shown to be simple, efficient and sensitive, and was suitable for the determination of these compounds in milk.

关 键 词：中空纤维液相微萃取 高效液相色谱 大环内酯类抗生素 替米考星 交沙霉素 麦迪霉素 牛奶 

分 类 号：TS252.7[轻工技术与工程—农产品加工及贮藏工程]