摘要
建立了米面制品中硫脲的液相色谱-串联质谱(LC-MS/MS)测定方法。实验优化了样品提取方法、液相色谱条件和质谱参数。样品用80%乙醇超声波提取,离子交换色谱分离,色谱柱为NUCLEOSIL100-5SA阳离子交换柱,流动相为乙腈-(1%乙酸+0.2%乙酸铵)水溶液(30:70),流速0.5mL/min。采用电喷雾质谱正离子模式电离,多反应选择离子检测,检测离子对为m/z77/60和m/z77/43,其中m/z77/60为定量离子对。结果表明:本方法简便快速、准确可靠,相对标准偏差<4.0%;回收率为83%～90%;检出限为0.5mg/kg;定量下限为5mg/kg。
A method was established for the determination of thiourea in noodle and rice flour using liquid chromatography-mass spectrometry（LC-MS/MS） in the multiple-reaction monitoring mode（MRM）.Thiourea was extracted by 80% ethanol with ultrasonic wave.The extract was separated on a cation ion exchange column（250 mm×4.6 mm,5 μm） with acetonitrile-（1% acetic acid ＋0.2% ammonium acetate）（70：30 by volume） as mobile phase at a flow rate of 0.5 mL/min and determined by positive ESI MS/MS.The conditions of extraction and LC-MS/MS were optimized.The parent ion of positive ESI MS was m/z 77,and the daughter ions of MS/MS were m/z 60 and 43.The MRM monitored ions,m/z 77/60 and m/z 77/43,were selected as qualitative ions,and m/z 77/60 was selected as quantitative ion.The recovery of thiourea was in the range of 83%-90% and the RSD was less than 4.0%.The limit of detection was 0.5 mg/kg.The method was proved to be simple and accurate.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2009年第10期1531-1534,共4页
Chinese Journal of Analytical Chemistry
基金
国标准化管理委员会资助项目(No.20071429-T-469)
关键词
硫脲
液相色谱
串联质谱
面条
米粉
Thiourea
liquid chromatography-mass spectrometry
noodle
rice flour
