CAJ | 학술논문

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。
건립업저육중라단명B잔류적미파췌취응효정화색보-초쾌속액상색보-천련질보（MAE-GPC-RRLC-MS/MS）적분석방법,채용다반응감측（MRM）소묘,정리자모식。양품경배기완-을산을지미파췌취제취、응효정화색보농축화정화후,이0.1%갑산수-갑순용액위류동상,경Agilent Plus C18주분리후진행RRLC-MS/MS다반응감측소묘모식분석검측。결과표명：업저육중라단명B적정량한위0.25μg/kg。재1.0、3.0、5.0μg/kg첨가수평하,상술라단명B적회수솔위71.1%～102.0%,상대표준편차위5.1%～17.1%。재1.0～100μg/L범위내,선성상관계수위0.9998。해방법구유쾌속、준학、특이성호등우점,가실현양본령민、준학적정성정량분석。
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.