首页> 中文期刊>肉类研究 >微波萃取-凝胶渗透色谱-超快速液相色谱-串联质谱法检测腌猪肉中的罗丹明B残留

微波萃取-凝胶渗透色谱-超快速液相色谱-串联质谱法检测腌猪肉中的罗丹明B残留

     

摘要

建立腌猪肉中罗丹明B残留的微波萃取凝胶净化色谱-超快速液相色谱-串联质谱(MAE-GPC-RRLC-MS/MS)的分析方法,采用多反应监测(MRM)扫描,正离子模式。样品经环己烷-乙酸乙酯微波萃取提取、凝胶净化色谱浓缩和净化后,以0.1%甲酸水-甲醇溶液为流动相,经Agilent Plus C18柱分离后进行RRLC-MS/MS多反应监测扫描模式分析检测。结果表明:腌猪肉中罗丹明B的定量限为0.25μg/kg。在1.0、3.0、5.0μg/kg添加水平下,上述罗丹明B的回收率为71.1%~102.0%,相对标准偏差为5.1%~17.1%。在1.0~100μg/L范围内,线性相关系数为0.9998。该方法具有快速、准确、特异性好等优点,可实现样本灵敏、准确的定性定量分析。%A new method is developed for the determination of rhodamine B residue in salted pork by microwave extraction- gel permeation chromatography-rapid resolution liquid chromatography-tandem mass spectrometry (MAE-GPC-RRLC-MS/ MS) with multiple reaction monitoring (MRM) in positive ionization mode. Samples were extracted with tert-butyl methyl ether under microwave assistance and then cleaned up by gel permeation chromatography. The chromatographic separation was performed on an Agilent Plus C18 column using a mobile phase consisting of 0.1% aqueous formic acid and methanol. The limit of quantification (LOQ) of the RRLC-MS/MS method was 0.25 lag/kg and the linear range was between 1.0 μg/L and 100 μg/L with a correlation coefficient of 0.9998. The recovery rates of rhodamine B at the spike levels of 1.0, 3.0 μ g/kg and 5.0 μ g/kg were in the range of 71.1% to 102.0% with relative standard deviation between 5.1% and 17.1%. This method had the advantages of rapidity, accuracy and specificity and allowed sensitive and accurate qualification and quantification of rhodamine B.

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