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固相萃取-高效液相色谱法测定牛乳中氯霉素残留 被引量:12

Determination of residue of chloramphenicol in bovine milk by solid phase extraction HPLC
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摘要 目的:建立简便、灵敏、准确的牛乳中氯霉素残留测定方法.方法:以非那西丁为内标,牛乳样品先采用10%高氯酸溶液沉淀蛋白,再经strata-X固相小柱萃取,洗脱液浓缩后在ODS(4.6×150 mm)柱上,以乙腈-5 mmol/L磷酸氢二铵缓冲溶液(22:78)为流动相,277 nm检测.结果:线性关系良好(r=0.9996),定量限(LOQ)为0.5 ng/ml,各浓度绝对回收率67.9%~77.6%,相对回收率85.4%~104.1%.结论:该方法简单、迅速、灵敏度高,适合用于牛乳中氯霉素的残留量的检测. Objective:To develop a method for determination of residue of chloramphenicol in bovine milk. Methods:The milk, containing phenacetin as internal standard, is deproteined with 10% HClO4 first. The supernatant is then extracted and condensed with strata - X column. The target elution is determined on ODS (6.0 × 150 mm) column with acetonitrile -5 mmol/L diammonium hydrogen phosphate (22:78 ) as mobile phase and with UV detector being set at 277 nm. Results:The calibration curve is linear over the range of 0. 532 - 10. 64 ng/ml. The limit of quantification was 0. 532 ng/ml. Extraction recovery and the method recovery were 67. 9% - 77. 6% and 85.4% - 104. 1% respectively. Conclusion:The method is sensitive, accurate and convenient and reliable to determinate the residue of chloramphenicol in bovine milk.
出处 《中国卫生检验杂志》 CAS 2005年第12期1426-1428,共3页 Chinese Journal of Health Laboratory Technology
基金 2004年中国药科大学青年教师科技基金项目(A0304)
关键词 氯霉素 牛乳 固相萃取 高效液相色谱法 Chloramphenicol Bovine milk Solid phase extraction HPLC
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