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柱前衍生高效液相色谱法测定猪肉中5种青霉素残留量
Determination of 5 Penicillin Residues in Pork by High Performance Liquid Chromatography with Pre-column Derivatization
【摘要】 样品采用乙腈直接提取 ,离心分离及用液 液分配和固相萃取 (C18柱 )净化方式 ,经衍生后 ,用液相色谱紫外检测器测定猪肉中 5种青霉素残留量。使用的分离柱是NovaPakC18柱 ,流动相为乙腈和磷酸盐混合液。方法检出限 0 .0 2mg/kg,回收率为 70 .9%~96.5% ,相对标准偏差为 3.1 0 %~ 6.71 %。
【Abstract】 A liquid chromatographic method (LC) with ultraviolet (UV) detection was developed for analysis of penicillin G,penicillin V, oxcillin, cloxacillin and dicloxacillin in pork. The sample was extracted with acetonitrile, followed by centrifuging precipitation , partition of liquid liquid and solid phase extraction, after derivatization with 1,2,4 triazole and HgCl 2 under heat, the product of derivatization was determined by reverse phase LC with UV detection. Waters Nova Pak C 18 (150×3.9mm i.d.) was used as separation column, and the mixture of acetonitrile and phosphate buffer was used as flow phase. The limits of detection were 0.02 mg/kg. Average recoveries of 5 penicillins were in the range of 70.9%~96.5% and the RSD were 3.1%~6.7%.
【Key words】 Penicillin; residue; high performance liquid chromatography; pork; pre column derivation;
- 【文献出处】 分析化学 ,Chinese Journal of Analytieal Chemistry , 编辑部邮箱 ,2001年07期
- 【分类号】O657.7
- 【被引频次】29
- 【下载频次】223