摘要
建立了动物组织中金霉素残留测定的高效液相色谱柱后衍生法,研究了镁离子和草酸体系对金霉素荧光强度的影响。结果表明,镁离子浓度和草酸浓度为1∶1.2时,金霉素的荧光强度最强。动物组织样品以5%高氯酸提取,正己烷脱脂,C18净化,Hy-persil ODS C18(250×4.6 mm,5μm)分离,流动相为甲醇∶0.05 mol/L草酸=80∶20(V/V),流速为0.7 mL/min,柱后0.05 mol/L乙酸镁衍生,流速为0.1 mL/min,紫外检测器和荧光检测器同时测定,提高了金霉素残留定量灵敏度。紫外检测波长365nm,荧光检测波长eλx=360 nm,eλm=520 nm。
An analytic method for the determination of chlortetracycline in animal tissue by HPLC/post column derivatization was developed. The characteristic fluorescence of chlortetracycline was investigated in the system of magnesium acetate and oxalic acid. When the concentration ratio of magnesium acetate and oxalic acid was 1 ： 1. 2, the fluorescence intensity of chlortetracycline was the maximum. The sample was extracted by 0.5% acetonitril, degreased by hexane, purified by SPE（C18） and separated with a Hypersil ODS C18（250×4.6 mm, 5 μm）. The mobile phase was methanol/0.05 mol/L oxalic acid （80 ： 20, V/V）, and the flow rate was set at 0. 7 mL/min. The post column derivatization reactions were performed with 0.05 mol/L magnesium acetate, and the flow rate was set at 0. 1 mL/min. Two detector of ultraviolet and fluorescence were used, which can improve the quantitative analysis of chlortetracycline residue. The detection wavelengths were set at 365 nm and λex /λem=360/520 nm, respectively.
出处
《分析科学学报》
CAS
CSCD
2008年第3期295-298,共4页
Journal of Analytical Science
基金
云南省农业科学院创新基金(2005012)
关键词
动物组织
金霉素
高效液相色谱
柱后衍生
荧光
Animal tissue
Chlortetracycline
HPLC
Post column derivatization
Fluorescence
