An MAE-GPC-RRLC-MS/MS Method for Quantitative Determination of Rhodamine B Residue in Salted Pork
LIU Hong-hua，ZHANG Li-kang，WU Wei，ZHANG Jing-xuan，ZHANG Yan
1. The Sixteenth Secondary School of Tangshan, Tangshan 063000, China；
2. Hebei Key Laboratory of Food Security, Hebei Institute of Food Quality Supervision Inspection and Research, Shijiazhuang
050091, China；3. Department of Life Sciences, Tangshan Normal University, Tangshan 063000, China
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。
Abstract：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.
刘宏华；张利康；武炜；张敬轩；张岩. 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[J]. 肉类研究, 2012, 26(5): 30-33.
LIU Hong-hua，ZHANG Li-kang，WU Wei，ZHANG Jing-xuan，ZHANG Yan. An MAE-GPC-RRLC-MS/MS Method for Quantitative Determination of Rhodamine B Residue in Salted Pork. Meat Research, 2012, 26(5): 30-33.
2012, Vol. 26 
