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目的研究有效提取和净化调味油中罗丹明B的两种前处理方法,为超高效液相色谱-荧光检测(UPLC-FLR)法的准确定量提供有价值的参考。方法第一种方法用酸化乙腈提取,混合型阳离子交换固相萃取(SPE)柱净化;第二种方法用含20%丙酮的正己烷提取,中性氧化铝SPE柱净化。两种方法的净化液吹至近干,用50%甲醇-水复溶,滤膜过滤后用UPLC-FLR测定。结果两种方法中罗丹明B在5.0、50.0、200.0μg/kg三个水平下的加标回收率分别在82.8%~101.9%、80.9%~93.6%之间,相应相对标准偏差(RSD)分别在1.5%~2.9%(n=6)、1.0%~2.1%(n=6)之间。结论两种方法均可满足调味油中罗丹明B的测定,第一种方法在5.0、50.0μg/kg加标水平的回收率均优于第二种方法,且无需大容量SPE柱;高浓度(200.0μg/kg)加标水平的回收率差异无统计学意义(P>0.05)。
OBJECTIVE To study two pretreatment methods for the effective extraction and purification of rhodamine B in flavoring oil, and to provide a valuable reference for the accurate quantification of UPLC-FLR. Methods The first method was extracted with acidified acetonitrile and mixed cation exchange solid phase extraction (SPE) column. The second method was extracted with n-hexane containing 20% acetone and neutral alumina SPE column. The two methods of purification solution were blown to near dryness, reconstituted with 50% methanol-water, filtered through a UPLC-FLR filter. Results The spiked recoveries of Rhodamine B at the concentrations of 5.0, 5.0 and 200.0 μg / kg were 82.8% -101.9% and 80.9% -93.6%, respectively, and the corresponding relative standard deviations (RSDs) were respectively Between 1.5% and 2.9% (n = 6) and between 1.0% and 2.1% (n = 6). Conclusion Both methods can meet the requirement of Rhodamine B in the flavoring oil. The first method is superior to the second method at the spiked levels of 5.0 and 50 μg / kg, (200.0μg / kg) spiked level of recovery was no significant difference (P> 0.05).