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机构地区:[1]温州大学生命与环境科学学院,浙江温州325027 [2]温州出入境检验检疫局,浙江温州325027
出 处:《中国食品学报》2009年第2期187-193,共7页Journal of Chinese Institute Of Food Science and Technology
摘 要: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.
关 键 词:苏丹红 对位红 气相色谱-质谱-选择离子检测 内标法
分 类 号:TS207.5[轻工技术与工程—食品科学]
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