【摘要】：[目的]為了解硫酸頭孢喹肟在雞蛋中的殘留,以確定蛋雞用藥的合理休藥期,建立了硫酸頭孢喹肟在雞蛋內的高效液相色譜(HPLC)殘留檢測方法。[方法]取空白雞蛋樣品,按質量體積比1∶19的比例添加相應濃度的硫酸頭孢喹肟對照品溶液制備生物樣品,用酸性乙腈提取藥物,正己烷分離脂肪,C18固相萃取小柱凈化洗脫后,洗脫液經(jīng)40℃水浴N2吹干濃縮后復溶,在紫外吸收波長270 nm下進行HPLC檢測。[結果]硫酸頭孢喹肟在0.02~2.00μg·m L~(-1)濃度范圍內線性關系良好,回歸方程為:y=164.95x+0.693(R2=0.999 8);方法的最低檢測限0.01μg·m L~(-1),定量限0.02μg·m L~(-1);藥物在生物樣品中的低、中、高濃度分別為0.01、0.10和1.00μg·m L~(-1)時,雞蛋中硫酸頭孢喹肟的回收率為85.6%~90.4%,變異系數(shù)為6.59%~10.47%,均在規(guī)定的藥物殘留檢測添加回收率和變異系數(shù)范圍內。此外,該檢測方法的特異性好、準確度高,24 h內生物樣品在室溫、4℃(冷藏)和-20℃(冷凍)條件下穩(wěn)定性均良好,且臨床常用抗菌藥物不存在干擾。[結論]經(jīng)方法學驗證,本方法適用于雞蛋中硫酸頭孢喹肟含量的檢測,可應用于臨床的生物樣品檢測。
[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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