超高效液相色谱-串联质谱测定面制品中的呋喃西林代谢物

Determination of Semicarbazide in Flour Products by Ultra Performance Liquid Chromatography-tandem Mass Spectrometry

摘要:

利用超高效液相色谱-电喷雾串联质谱（UPLC-ESI-MS/MS）方法测定了面制品中的呋喃西林代谢物-氨基脲（SEM）。样品经0.2mol/L的盐酸溶液均质，2-硝基苯甲醛衍生化，乙酸乙酯提取浓缩后，经固相萃取（SPE）柱净化，采用BEH C18柱分离，以乙腈和0.1% (V/V)的甲酸水溶液为流动相进行梯度洗脱，采用正离子、多反应监测(MRM)模式进行定性定量测定。结果表明弱阳离子交换柱的净化效果较好，氨基脲在1~100 μg/kg质量浓度范围内线性关系良好，相关系数r为0.9993；检出限为0.4 μg/kg。添加水平分别为2、10、50 μg/kg时的加标回收率为85.8%~112.6%，相对标准偏差小于9%。本方法适用于不同面制品中氨基脲的定性和定量分析。

Abstract:

A method was developed for the determination of semicarbazide in flour products based on solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry (SPE-UPLC-MS/MS ) in the article．The samples were homogenized with 0.2mol/L HCl, derivatized with 2-notrobenzaldehyde, and the derivative was extracted with ethyl acetate. The extract was cleaned up by a solid phase extraction cartridge. The target analytes were separated on a UPLC BEH C18 column with gradient elution using acetonitrile and water containing 0.1% (V/V) formic acid as mobile phase. The identification and quantification were achieved by using ESI-MS/MS in positive ion mode and with multiple reactions monitoring (MRM). The linear range was from 1 to 100 μg /kg with the correlation coefficient r=0.9993 for semicarbazide. The limit of detection (LOD) was 0.4 μg/kg. The recoveries of the method were ranged from 85.8% to 112.6% at the spiked levels of 2, 10, 50μg /kg and the relative standard deviation was less than 9%. The method was suitable for the qualitative and quantitative of semicarbazide in different flour products.