高效液相色谱法比较3种固相萃取柱净化对乳品中8种抗生素残留检测的影响  

Effects of Three Kinds of Solid Phase Extraction Columns Purification Methods on Determination of 8 Antibiotics Residues in Dairy by High Performance Liquid Chromatography

作　　者：刘彦东[1] 张权[1] 陈文生[1] 洪亮[1] 

机构地区：[1]贵州师范大学贵州省山地环境信息系统与生态保护重点实验室,分析测试中心,贵州贵阳550001

出　　处：《分析测试学报》2015年第3期362-366,共5页Journal of Instrumental Analysis

基　　金：贵州省科技厅科学技术基金项目(黔科合J字LKS[2011]31号)

摘　　要：对比了3种固相萃取柱(HLB柱、C18柱和PEP柱)对复杂乳品基质中目标物检测的影响,并建立了同时测定乳品中四环素类、β-内酰胺类及氯霉素等8种抗生素残留的固相萃取/高效液相色谱法。结果表明:HLB固相萃取柱的洗脱及净化效果较好,适用于复杂乳品基质的洗脱净化。在优化条件下,8种抗生素在5.0~100.0μg/L浓度范围内的线性关系良好(r2>0.999),检出限为0.09~0.84μg/kg,定量下限为0.32~2.23μg/kg。8种抗生素在不同加标浓度下(5,10,30μg/kg)的回收率为73.2%~93.3%,相对标准偏差(n=5)为1.4%~3.6%。研究结果表明,该方法适用于复杂乳品基质中8种不同种类抗生素的同时检测。The purified performance of three different types of solid-phase extraction columns, inclu- ding HLB column, C^s column and PEP column, was investigated in this study. And based on that, a solid phase extraction/high performance liquid chromatography was developed for the simultaneous determination of 8 antibiotic residues in dairy. The result indicated that the HLB column showed an excellent elution and purification effect, and it was applicable for the dairy matrix purification. Un- der the optimal conditions, the calibration curves of eight antibiotics were linear in the concentration range of 5.0 - 100.0 μg/L with correlation coefficients（r2） more than 0. 999. The limits of detection （LOD） and limits of quantitation（LOQ） of 8 antibiotics were in the range of 0. 09 - 0. 84 μg/kg and 0. 32 -2.23 μg/kg, respectively. The recoveries of target compounds at spiked concentration levels of 5, 10 and 30 μg/kg ranged from 73.2% to 93.3% , with relative standard deviations（n =5） of 1.4% - 3.6% . The developed method was suitable for the analysis of antibiotic residues in the com- plex dairy matrix.

关 键 词：高效液相色谱(HPLC) 固相萃取(SPE) 乳品 抗生素残留 净化 

分 类 号：O657.63[理学—分析化学] R978.1[理学—化学]