食品中苏丹红Ⅰ～Ⅳ及对位红的GC-MS／SIM法研究

Study on Simultaneous Determination of SudanⅠ～ SudanⅣ and Para Red in Food by GC-MS/SIM

目的：建立同时测定食品中苏丹红Ⅰ-Ⅳ及对位红的新方法。方法：采用气相色谱-质谱选择离子检测法，样品处理采用超声波直接提取和过中性氧化铝柱净化的方法，色谱柱为J＆W DB-5HT30．0m×250μLm×0．10μm石英毛细管柱，柱温的调节采用程序升温法。进样方式：脉冲不分流，进样量1μL；EI离子源，选择m/z248、143、115、276、247、105、293、171、352、380、261、225，利用选择离子法，以菲-氘10为内标进行研究。结果：苏丹红Ⅰ～Ⅳ及对位红的线性范围为0．1～4．0mg／L；方法检出限为0．002～0．01μg/g。RSD为3．7％～8．1％，回收率为82．2％～89．3％。结论：本试验结果准确可靠，选择性和重复性好。

Objective： To establish a new method for simuhaneous detecting Sudan I-SudanlV and para red in food. Methods：Gas chromatography-mass spectrum with selected ion monitor（GC-MS/SIM） was used. The sample was treated by combined Ultrasonic Extraction with the Alumina Column Purification. The chromatography column was J＆W DB-SHT （30.0 m×250 μm×0.10 μm） quartz capillary column. The procedure of GC was： 180℃ retain 3min, rise to 200℃ at 10℃/min and hold for 2 min, then rose to 320℃ at 20 ℃/min and retain 7min.The sampling method was not segregation, the amount of sample was 1μL. The EI ion source was used. The conditions of GC-MS were optimized, and the selected ions were m/z 248,143,115,276,247,105,293,171,352,380,261,225,respectively, according to the selected ions, integrating the apex area and analyzing the target objects with the inner standard （Phenanthrene-d10）. Results： The line or range of the determination Sudan Ⅰ～Ⅳ and para red was 0.01-4.0 mg/L with a detection limit of 0.002-0.01 μg/g. The recovery was 82.2%-89.3% and the RSD was 3.7%-8.1%. Conclusion： The method has been proved to be reliable, accurate and repeat and the results obtained were satisfactory.