鸡蛋中硫酸头孢喹肟残留的高效液相色谱检测方法的建立

发布时间：2019-03-20 11:28

【摘要】：[目的]为了解硫酸头孢喹肟在鸡蛋中的残留,以确定蛋鸡用药的合理休药期,建立了硫酸头孢喹肟在鸡蛋内的高效液相色谱(HPLC)残留检测方法。[方法]取空白鸡蛋样品,按质量体积比1∶19的比例添加相应浓度的硫酸头孢喹肟对照品溶液制备生物样品,用酸性乙腈提取药物,正己烷分离脂肪,C18固相萃取小柱净化洗脱后,洗脱液经40℃水浴N2吹干浓缩后复溶,在紫外吸收波长270 nm下进行HPLC检测。[结果]硫酸头孢喹肟在0.02~2.00μg·m L~(-1)浓度范围内线性关系良好,回归方程为:y=164.95x+0.693(R2=0.999 8);方法的最低检测限0.01μg·m L~(-1),定量限0.02μg·m L~(-1);药物在生物样品中的低、中、高浓度分别为0.01、0.10和1.00μg·m L~(-1)时,鸡蛋中硫酸头孢喹肟的回收率为85.6%~90.4%,变异系数为6.59%~10.47%,均在规定的药物残留检测添加回收率和变异系数范围内。此外,该检测方法的特异性好、准确度高,24 h内生物样品在室温、4℃(冷藏)和-20℃(冷冻)条件下稳定性均良好,且临床常用抗菌药物不存在干扰。[结论]经方法学验证,本方法适用于鸡蛋中硫酸头孢喹肟含量的检测,可应用于临床的生物样品检测。
[Abstract]:[objective] in order to understand the residues of cefquinoxime sulfate in eggs and to determine the reasonable withdrawal period of cefquinoxime sulfate in eggs, a high performance liquid chromatography (HPLC) (HPLC) method was established for the determination of cefquinoxime sulfate residues in eggs. [methods] the blank egg samples were prepared by adding the corresponding concentration of cefquinoxime sulfate reference solution to the ratio of mass to volume 1:19. The drug was extracted by acid acetonitrile and the fat was separated by n-hexane. C _ (18) solid-phase extraction column was used to purify and elute the eluent. The eluent was concentrated by N _ 2 blowing-drying at 40 鈩，

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