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BEHC18柱分离，以乙腈和0．1％（V/V）功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1－100μg／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0．49g／kg。添加水平分别为2、10、50Mg／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。
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 acetouitrile 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 ~tg/kg with the correlation coefficient r=0.9993 for semicarbazide. The limit of detection （LOD） was 0.4 btg/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.
出处
《现代食品科技》
EI
CAS
北大核心
2013年第2期416-421,共6页
Modern Food Science and Technology
基金
广东省质量技术监督局科技项目(2010ZB02)
关键词
超高效液相色谱-串联质谱
固相萃取
氨基脲
面制品
ultra performance liquid chromatography-tandem mass spectrometry
solid-phase extract
semicarbazide
flour products
