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建立高效液相色谱荧光检测法同时检测鸡组织中阿莫西林和氨苄西林残留的方法。鸡组织样品经磷酸二氢钠溶液提取,乙腈去蛋白,正己烷脱脂,饱和二氯甲烷萃取,上清液经水杨醛在酸性条件下沸水浴衍生化。以C18柱为固定相、0.01 mol/L的磷酸二氢钾溶液和乙腈溶液为流动相,梯度洗脱,流速为1 m L/min,荧光检测激发波长为358 nm,发射波长为440 nm。阿莫西林和氨苄西林在25~1 000μg/kg体重范围内线性关系良好,相关系数均大于0.9994。当阿莫西林和氨苄西林添加水平在10~100μg/kg体重时,鸡组织样品中平均回收率均高于68.65%,相对标准偏差均低于10.74%。阿莫西林、氨苄西林在鸡组织中的检测限均分别为5、3.5μg/kg体重,阿莫西林、氨苄西林的定量限均分别为13、10μg/kg体重。该方法灵敏、准确、快速,适用于鸡组织中阿莫西林、氨苄西林残留的同时检测。
To establish a method for simultaneous determination of amoxicillin and ampicillin residues in chicken tissues by high performance liquid chromatography with fluorescence detection. The chicken tissue samples were extracted with sodium dihydrogen phosphate solution, deproteinized with acetonitrile, defatted with n-hexane and extracted with saturated dichloromethane. The supernatant was derivatized with salicylaldehyde in a boiling water bath under acidic conditions. The C18 column was used as the stationary phase. The mobile phase was 0.01 mol / L potassium dihydrogen phosphate solution and acetonitrile. The gradient elution was performed at a flow rate of 1 mL / min. The excitation and emission wavelengths were 358 nm and 440 nm respectively. Amoxicillin and ampicillin had a good linear relationship in the range of 25-1 000 μg / kg body weight with the correlation coefficients greater than 0.9994. When the amoxicillin and ampicillin levels were 10 ~ 100μg / kg body weight, the average recovery of chicken tissue samples were higher than 68.65%, the relative standard deviations were less than 10.74%. The limits of detection of amoxicillin and ampicillin in chicken tissues were 5 and 3.5 μg / kg body weight respectively. The limits of quantification for amoxicillin and ampicillin were 13 and 10 μg / kg body weight, respectively. The method is sensitive, accurate and rapid and suitable for the simultaneous detection of amoxicillin and ampicillin residues in chicken tissues.