摘要
采用气相色谱-质谱(GC-MS)选择离子检测法(SIM),建立了准确可靠、灵敏度高、快速简便的同时测定食品中苏丹红Ⅰ~Ⅳ的新方法.色谱柱为PR-SR石英毛细管柱(20 m×0.25 mm),进样口温度280℃,柱温200℃,以15℃/min升至280℃;柱前压130 kPa,载气He;EI离子源,选择m/z 77,105,115,143,176,247,248,261,352,380用于SIM检测,并按不同的采样时间分成4组,每组4个离子,分别对应于每种苏丹红进行定性分析确证;选择苏丹红Ⅰ~Ⅳ各自的分子离子峰m/z 248,276,352,380作抽出离子图进行定量分析.苏丹红Ⅰ、Ⅱ的线性范围为0.01~10.0 mg/L,苏丹红Ⅲ、Ⅳ的线性范围为0.1~10.0 mg/L;检出限苏丹红Ⅰ、Ⅱ为1μg/kg,苏丹红Ⅲ为5μg/kg,苏丹红Ⅳ为10μg/kg;回收率86%~95%.本法与欧洲健康与消费者保护委员会的方法(HPLC法)相比灵敏度高1~2个数量级,分析时间缩短,用色谱保留时间、质谱同时定性,消除了食品中杂质的干扰,结果准确可靠,选择性和重复性好,适用于所有食品成品及原料的检验.
A new method was established for determining SudanⅠ-Ⅳin food by gas chromatography-mass spectrum with selected ion monitor(GC-MS/SIM).The conditions of GC-MS were optimized,and the selected ions were m/z77,105,115,143,176,247,248,261,352,380,respectively.The interfer-ences caused by the impurities in food could be avoided by this method.The linear range of the determination SudanⅠandⅡwere0.01-10mg/Lwith a determination limitof1μg/kg.The linear range of the determi-nation SudanⅢandⅣwere0.1-10mg/L with a determination limit of5and10μg/kg.The recovery range was86%-95%and the RSD was less than6.1%.The method has been proved to be reliable and accurate.It has been applied to the determination of SudanⅠ-Ⅳin food with satisfactory results.
出处
《分析测试学报》
CAS
CSCD
北大核心
2005年第4期1-5,共5页
Journal of Instrumental Analysis
关键词
苏丹红
食品
气相色谱-质谱
选择离子检测
SudanⅠ-Ⅳ
Food
Gas chromatography-Mass spectrum
Select ion monitor