摘要: |
建立高效液相色谱荧光法检测鸡组织中阿莫西林的残留量。鸡组织样品经磷酸二氢钠溶液提取,乙腈去蛋白,正己烷去脂肪,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0.01 mol.L-1的磷酸二氢钾溶液(A)和乙腈溶液(B)为流动相,梯度洗脱,流速为1mL.min-1,高效液相色谱荧光检测,激发波长为358nm,发射波长为440nm。阿莫西林在25~1000μg.kg-1质量浓度范围内,线性关系良好。当阿莫西林添加水平为13~125μg.kg-1时,鸡组织中AMO的平均回收率在72.82%~88.82%,相对标准偏差在6.21%~9.63%;检测限、定量限分别为5μg.kg-1(S/N≥3)、13μg.kg-1(S/N≥10)。该方法操作简便,可适用于鸡组织中阿莫西林的提取和检测,且准确度和精密度均符合残留分析的要求。 |
关键词: 高效液相色谱 阿莫西林 荧光检测法 鸡组织 |
DOI: |
投稿时间:2014-07-25修订日期:2014-08-28 |
基金项目:山东出入境检验检疫局科技项目(SK201349);国家肉鸡产业技术体系专项(CARS-42-G23) |
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Determination of residues of amoxicillin in chicken tissues by HPLC with fluorescence detection |
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(Weifang Entry-Exit Inspection And Quarantine Bureau) |
Abstract: |
To develop a high performance liquid chromatography with fluorescence detection (HPLC-FLD) method for determination of residues of amoxicillin (AMO) in chicken tissues. AMO were extracted from chicken tissues with sodium dihydrogen phosphate solution. After being deproteinizated with acetonitrile and degreased in n-hexane saturated, the analyte was extracted by saturated dichloromethane. The supernatant was reacted with salicylaldehyde under acidic and boiling conditions. The mobile phase were 0.01M potassium dihydrogen phosphate(A) and acetonitrile (B), the flow rate was 1mL.min-1. Fluorescence detection was carried out at excitation and emission wavelengths of 358nm and 440nm.The calibration curves were linear in the range from 25 to 1000μg.kg-1. At spiked level 13~125μg.kg-1 for AMO, the average recoveries was 72.82%~88.82% with coefficients of variation between 6.21% and 9.63%. Limit of detection (LOD) and limit of quantitation (LOQ) were 5μg.kg-1 and 13μg.kg-1, respectively. This HPLC-FLD method is simple, rapid, sensitive and reliable for the determination of residues of amoxicillin in chicken tissues. |
Key words: HPLC amoxicillin (AMO) fluorescence detection chicken tissue |