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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: To establish a method for the simultaneous determination of Sudan Ⅰ, Ⅱ, Ⅲ and Ⅳ in chili oil by gel permeation chromatography (GPC) and UPLC-MS / MS. Methods: The sample was dissolved in cyclohexane / ethyl acetate 1/1 (V / V) and the oil was removed by GPC gel permeation chromatography. The sample was determined by UPLC-MS / MS. Results: Quantitative using external standard method. The detection limits of Sudan Ⅰ, Ⅱ, Ⅲ and Ⅳ in chili oil were 6 ng / kg, 0.6 ng / kg, 0.06 ng / kg and 120 ng / kg, respectively. The spiked recoveries ranged from 88.1% to 110.7% for Sudan Ⅰ, 88.1% to 119.6% for Sudan Ⅱ, from 98.1% to 118.2% for Sudan Ⅲ, and from Sudan Ⅳ : 75.7% ~ 115.6%, RSD 1.28% ~ 5.19%. Conclusion: The method has the advantages of simple sample preparation, reliable purification method, good selectivity, high sensitivity and good reproducibility.