摘要
建立液相色谱—质谱法测定氯霉素残留量,以淡水鱼为分析对象,通过优化前处理、色谱质谱条件等因素测定淡水鱼中氯霉素残留量,样品经制备、提取、净化、氮吹复溶后由高效液相色谱—质谱联用仪检测,采用多反应监测(MRM)模式测定。根据保留时间和特征离子对的相对丰度比定性,内标法定量。标准品在质量浓度0.25~10μg·L^(-1),分析结果峰面积呈现良好的线性关系,相关系数0.9993;本方法选用低中高3个加标质量浓度:0.5,2,5μg·L^(-1),各自平行加标6次,得到平均回收率为90.0%~101.2%,RSD为1.2%~5.8%,检出限通过11次质量浓度为0.25μg·L^(-1)标准溶液加标峰面积计算标准偏差,以3倍标准偏差与平均峰面积比值计算,检出限为0.033μg·kg^(-1),定量限为0.10μg·kg^(-1)。在该方法采样的色谱—质谱条件下进行检测,有操作简单、灵敏度高、结果准确、迅捷等优点,可用于对淡水鱼中氯霉素的检测。
A liquid chromatography-mass spectrometry(LC-MS)method for the determination of chloramphenicol residues was established,with freshwater fish as the analytical target.The residual amount of chloramphenicol in freshwater fish was determined by optimizing factors such as pretreatment,chromatographic and mass spectrometric conditions.The samples were prepared,extracted,purified,redissolved after nitrogen blowing,and then subjected to detection by high-performance liquid chromatography-mass spectrometry.The multiple reaction monitoring(MRM)mode was adopted for determination.Qualitative analysis was based on retention time and the relative abundance ratio of characteristic ion pairs,and quantitative analysis was conducted using the internal standard method.The standard substances within the volume concentration range of 0.25~10μg·L^(-1)exhibited a favorable linear relationship in the analysis result peak area,with a correlation coefficient of 0.9993.In this method,six spiking concentration levels,namely low,medium,and high(0.5,2 and 5μg·L^(-1)),were selected,and each was spiked in parallel three times.The average recovery rate ranged from 90.0%~101.2%,and the RSD was 1.2%~5.8%.The detection limit was calculated by computing the standard deviation of the peak area from 11 spiked standard solutions with a concentration of 0.25μg·L^(-1),and the ratio of three times the standard deviation to the average peak area.The detection limit was 0.033μg·kg^(-1),and the quantitative limit was 0.10μg·kg^(-1).Under the chromatography-mass spectrometry conditions adopted in this method for detection,it possesses advantages such as simple operation,high sensitivity,accurate results,and rapidity,and can be applied for the detection of chloramphenicol in freshwater fish.
作者
黄藤波
陈纯
黄国春
林泽鹏
罗炜雄
HUANG Tengbo;CHEN Chun;HUANG Guochun;LIN Zepeng;LUO Weixiong(Guangdong Jianxun Testing Technology Co.,Ltd.,Dongguan523857,China;Shenzhen Yiteng Testing Technology Co.,Ltd.,Shenzhen518105,China;Guangzhou Fu'an Testing Technology Co.,Ltd.,Guangzhou510555,China)
出处
《山东化工》
2025年第15期124-126,135,共4页
Shandong Chemical Industry
关键词
淡水鱼
氯霉素
液相色谱—质谱法
freshwater fish
chloramphenicol
liquid chromatography-mass spectrometry
