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作 者:张惠艳[1] 李艳菊[1] 顾金刚[2] 肖思颖[1]
机构地区:[1]北京理工大学生命学院,北京100081 [2]中国农业科学院农业资源与农业区划研究所,北京100081
出 处:《分析试验室》2014年第10期1130-1134,共5页Chinese Journal of Analysis Laboratory
基 金:国家863项目(2013AA102805-05)资助
摘 要:建立了高效液相色谱法检测生物降解药渣中残留金霉素的定量分析方法。药渣经EDTA-Mcllvaine缓冲液辅助超生波提取,用C18(3μm,4.6×150mm)反相色谱柱,A相为0.1%甲酸水溶液,B相为V(甲醇):V(乙腈)=2:3,V(A):V(B)=2:1进行洗脱,通过二极管阵列检测器在375 nm检测,金霉素与其它物质的峰能够完全分离。在1.0-1500.0 mg/L范围内,金霉素标准曲线R2为0.9991,检出限为3.0μg/kg,加标回收率在94%-102%之间,相对标准偏差为2.1%-7.7%。A method for the determination of chlortetracy cline content in its extracted residue by highperformance liquid chromatography (HPLC) was developed. The chlortetracycline was extracted with EDTA- Mcllvaine buffer, and tested at 375 nm on a diode array detector with a reversed-phase column of C18 (3 μm,4. 6× 150 mm). The aqueous phase filled with formic acid (0. 1% ) and the organic phase filled with V(methanol)/ V(acetonitrile) = 2 : 3, V ( A ) : V ( B ) = 2 : 1. The peaks of chlortetracycline and related substances can be completely separated. The linear range over chlotetracycline hydrochloride concentration was 1.0 - 1500. 0 mg/L with the correlation coefficient R2 of 0. 9991, detection limit was 3.00μg/kg, recoverieswere in 94% - 102% , relative standard deviations (RSD) were from 2. 1% to 7.7%. The method is simple, accurate and reliable, and could be used to determine residue levels of chlortetracycline hydrochloride.
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