Xie Kaizhou, Jia Longfei, Xu Dong, Guo Huisheng, Xie Xing, Huang Yuping, Chen Xuesen, Bao Wenbin, Dai Guojun, Wang Jinyu
College of Animal Science and Technology, Yangzhou University, Yangzhou 225009, People's Republic of China.
J Chromatogr Sci. 2012 Aug;50(7):620-4. doi: 10.1093/chromsci/bms052. Epub 2012 May 3.
A sensitive and robust method is presented for the simultaneous determination of amoxicillin (AMO) and ampicillin (AMP) in eggs by reversed-phase high-performance liquid chromatography with fluorescence detection (RP-HPLC-FLD). This method used a simple liquid-liquid extraction of the samples with acetonitrile and dichloromethane as precipitation of proteins and extraction solvent. AMO and AMP reacted with salicylaldehyde to form fluorescent derivatives, which were then analyzed with RP-HPLC-FLD. Separation was carried out on an Athena C18 column with a mobile phase consisting of 0.01 M potassium dihydrogen phosphate, adjusted to pH 5.5 by 2M potassium hydroxide and acetonitrile. The detector response was linear over the tested concentration range from 5.0 to 800 ng/mL for AMO and AMP. The recovery values ranged from 78.4 to 88.7% for AMO and from 77.6 to 82.0% for AMP. The limits of detection were 1.2 for AMO and 0.4 µg/kg for AMP. The limits of quantification were 3.9 for AMO and 1.5 µg/kg for AMP. The corresponding intra-day and inter-day variation (relative standard deviation) were found to be less than 9.6 and 14.8%, respectively.
建立了一种灵敏且稳健的反相高效液相色谱-荧光检测法(RP-HPLC-FLD),用于同时测定鸡蛋中的阿莫西林(AMO)和氨苄西林(AMP)。该方法采用简单的液-液萃取,以乙腈和二氯甲烷作为蛋白质沉淀剂和萃取溶剂。AMO和AMP与水杨醛反应形成荧光衍生物,然后用RP-HPLC-FLD进行分析。在Athena C18柱上进行分离,流动相由0.01 M磷酸二氢钾组成,用2M氢氧化钾调节至pH 5.5,并加入乙腈。在5.0至800 ng/mL的测试浓度范围内,AMO和AMP的检测器响应呈线性。AMO的回收率为78.4%至88.7%,AMP的回收率为77.6%至82.0%。AMO的检测限为1.2 μg/kg,AMP的检测限为0.4 μg/kg。AMO的定量限为3.9 μg/kg,AMP的定量限为1.5 μg/kg。相应的日内和日间变化(相对标准偏差)分别小于9.6%和14.8%。