摘要
目的:建立了用凝胶渗透色谱(GPC)净化,并用超高效液相色谱-串联质谱(UPLC-MS/MS)同时检测辣椒油中苏丹红Ⅰ、Ⅱ、Ⅲ、Ⅳ的方法。方法:样品经环己烷/乙酸乙酯1/1(V/V)溶解,经GPC凝胶渗透色谱除去油脂,UPLC-MS/MS测定。结果:采用外标法定量。辣椒油中苏丹红Ⅰ、Ⅱ、Ⅲ、Ⅳ的检出限分别为:6 ng/kg、0.6ng/kg、0.06 ng/kg、120 ng/kg。当添加浓度在1μg/kg^10μg/kg时,其加标回收率范围为:苏丹Ⅰ:88.1%~110.7%;苏丹Ⅱ:88.1%~119.6%;苏丹Ⅲ:98.1%~118.2%;苏丹Ⅳ:75.7%~115.6%,RSD为1.28%~5.19%。结论:本方法具有样品前处理简单、净化方法可靠、选择性好、灵敏度高、重现性好等特点。
Objective: A high sensitive and rapid method for simultaneous determination of sudan Ⅰ、Ⅱ、Ⅲ、Ⅳ in chili oil was established based on gel permeation chromatography ( GPC ) cleanup followed by ultra - perform- ance liquid chromatography tandem mass spectrometry detection. Methods: The samples were dissolved by cyclo- hexane/ethyl acetate 1/1 (V/V) and cleaned up by gel permeation chromatograph, finally determined by ultra- performance liquid chromatography tandem mass spectrometry. Results : Quantitative analysis of four kinds of sudans was carried out by external standard. The detection limits of sudan Ⅰ、Ⅱ、Ⅲ、Ⅳ were 6 ng/kg, 0.6 ng/kg, 0.06 ng/kg, 120 ng/kg, respectively. At concentration of 1 μg/kg - 10μg/kg, the average recoveries of sudan Ⅰ ranged from 88.1%-110.7%, sudan Ⅱ: 88.1% -119.6%, sudan Ⅲ: 98.1% -118.2%, sudan Ⅳ: 75.7% 115.6%, and the RSDs were 1.28% -5.19%. Conclusion: This developed analytical method with simple pre- treatment provided high sensitivity, selectivity, efficiency and repeatability.
出处
《中国卫生检验杂志》
北大核心
2013年第8期1875-1878,共4页
Chinese Journal of Health Laboratory Technology
关键词
凝胶渗透色谱
超高效液相-串联质谱
苏丹红Ⅰ
苏丹红Ⅱ
苏丹红Ⅲ
苏丹红Ⅳ
辣椒油
Gel permeation chromatograph ( GPC )
Ultra - performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS)
Sudan Ⅰ
Sudan Ⅱ
Sudan Ⅲ
Sudan Ⅳ
Chili oil
作者简介
黄希汇(1988-),女,本科,技师,主要从事理化检验工作。