摘要
建立基于QuEChERS净化提取的液相色谱-串联质谱法测定鸡蛋中氟苯尼考、金刚烷胺和金刚乙胺的检测方法。样品经含1%甲酸的乙腈-水(体积比为80∶20)溶液提取,用QuEChERS净化管净化,采用Agilent EC-C_(18)(100 mm×3.0 mm,2.7μm)色谱柱分离,以0.2%甲酸水溶液和甲醇作为流动相,梯度洗脱,正负离子切换模式下检测,金刚烷胺与金刚乙胺用同位素内标法定量,氟苯尼考用外标法定量。氟苯尼考的色谱峰面积与质量浓度在0.5~20 ng/mL范围内呈现良好的线性关系,相关系数为0.998;金刚烷胺和金刚乙胺的色谱峰面积与内标色谱峰面积的比值与质量浓度在0.5~20 ng/mL范围内呈现良好的线性关系,相关系数分别为0.9991和0.9996。氟苯尼考、金刚烷胺和金刚乙胺的检出限均为1.0μg/kg。空白样品在高、中、低3种加标浓度水平时的平均回收率为84.0%~117.9%,测定结果的相对标准偏差为5.6%~12.0%(n=6)。该方法满足鸡蛋中氟苯尼考、金刚烷胺和金刚乙胺同时测定的要求。
A method for the determination of florfenicol,amantadine and rimantadine in eggs by liquid chromatography-tandem mass spectrometry based on QuEChERS purification and extraction was established.The sample were extracted by acetonitrile aqueous solution(volume ratio was 80∶20)containing 1%formic acid,purified with QuEChERS purification tube,Separated through Agilent EC-C_(18)(100 mm×3.0 mm,2.7μm)chromatographic column,detected under positive and negative ion switching mode with 0.2%formic acid aqueous solution and methanol used as mobile phase to gradient elution.Amantadine and rimantadine were quantified by isotope internal standard method,and florfenicol was quantified by external standard method.The chromatographic peak area of florfenicol had a good linear relationship with the mass concentration in the range of 0.5-20 ng/mL,and the correlation coefficient was 0.998;The ratio of chromatographic peak area to internal standard chromatographic peak area of amantadine and rimantadine had a good linear relationship with the mass concentration in the range of 0.5-20 ng/mL,and the correlation coefficients were 0.9991 and 0.9996 respectively.The detection limits of florfenicol,amantadine and rimantadine were all 1.0μg/kg.The average recoveries of blank samples at high,medium and low spiked levels were 84.0%-117.9%,and the relative standard deviations of the determination results were 5.6%-12.0%(n=6).The method can meet the requirements of simultaneous determination of florfenicol,amantadine and rimantadine in eggs.
作者
倪炜华
陈妍
王丽丽
薛羽晴
NI Weihua;CHEN Yan;WANG Lili;XUE Yuqing(Jiaxing Institute for Food and Drug Control and Product Quality,Jiaxing 314000,China;North Minzu University Biological Science and Engineering College,Yinchuan 750030,China)
出处
《化学分析计量》
CAS
2022年第3期31-35,共5页
Chemical Analysis And Meterage
