制备了一种新型的聚苯乙烯纳米纤维,将其作为固相萃取吸附剂装填制成固相萃取柱,与高效液相色谱联用建立了干辣椒、水果饮料及红酒中罗丹明B的定量分析方法.高效液相色谱以3 g/L磷酸缓冲液-甲醇混合溶液(体积比3∶7,pH=7.0)为流动相.通过对提取条件的优化,得到该方法对干辣椒中罗丹明B的检出限为0.1 ng/g,最低定量限为0.6 ng/g;对水果饮料和红酒中罗丹明B的检出限均为0.2 ng/m L,最低定量限均为0.5 ng/m L.此方法对干辣椒中罗丹明B的提取回收率为98.2%~110.3%;对水果饮料中罗丹明B的提取回收率为94.6%~102.2%;对红酒中罗丹明B的提取回收率为90.4%~104.6%.该方法的线性范围为1~100 ng/m L(ng/g),相对标准偏差为2.3%~9.0%.该方法灵敏度高、选择性好,可用于干辣椒、水果饮料及红酒中罗丹明B的定量分析.
A method for the determination of Rhodamine B in dry chilli, fruit drink and red wine was developed and validated. The analyte was extracted with acetonitrile from foodstuffs. A novel electrospun polymer nanofibers packed micro-column was used for cleaning and concentrating the Rhodamine B in these foodstuffs. High performance liquid chromatography with fluorescence detection (HPLC-Flu) was used for the determination of Rhodamine B in the samples. The mobile phase was composed of 3 g/L phosphate buffer and methanol( 3 : 7, volume ratio) , the pH was adjusted to 7.0 with orthophosphoric acid. The results showed that the standard curve was linear over the validated concentrations range of 1-100 ng/mL( ng/g), and the limit of detection (LOD) for Rhodamine B spiked samples was 0. 1 ng/g in dry chilli, 0. 2 μg/mL in both fruit drink and red wine. The limit of quantitation ( LOQ ) for Rhodamine B spiked into dry chilli was 0. 6 ng/g, fruit drink 0. 5 ng/mL and red wine 0. 5 ng/mL, respectively. The average recoveries of Rhodamine B were 98.2%-110. 3% for dry chilli, 94. 6%-102. 2% for fruit drink, and 90. 4%-104. 6% for red wine, respectively. The relative standard deviation of the method was 2. 3%-9. 0%. This proposed method was applied to real samples including dry chilli, fruit drink as well as red wine, and there was no Rhodamine B found in fruit drink or red wine, but Rhodamine B was found in chilli powder.