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目的建立固相萃取-高效液相色谱-荧光检测法测定辣椒制品中罗丹明B的分析方法。方法样品分别经乙腈和20%丙酮-正己烷溶液提取后,采用Welchrom~P-SCX强阳离子交换固相萃取小柱和Welchrom~中性氧化铝固相萃取小柱进行净化,并采用Welch Ultimate~XB-C18色谱柱(250 mm×4.6 mm,5μm)以75%甲醇-水溶液为流动相进行分离,荧光检测器检测。结果采用Welchrom~P-SCX强阳离子交换小柱对辣椒制品进行前处理净化具有去除杂质效果更好,稳定性更强,方法重现性更好等优势,因而采用Welchrom~P-SCX小柱对辣椒制品进行前处理净化。罗丹明B在1.0~100.0μg/L范围具有良好的线性(r~2>0.9995),2种辣椒制品的回收率在91.4%~106.5%范围内,相对标准偏差RSD在2.1%~4.3%之间。结论该方法的灵敏度、准确度和精密度均符合罗丹明B的检测技术要求,且简便快速,适用于辣椒制品中罗丹明B的准确测定。
OBJECTIVE To establish a method for the determination of rhodamine B in pepper products by solid-phase extraction and high performance liquid chromatography-fluorescence detection. Methods The samples were extracted with acetonitrile and 20% acetone-n-hexane, respectively. The samples were purified by Welchrom ~ P-SCX strong cation exchange column and Welchrom ~ neutral alumina solid phase extraction cartridges. Ultimate ~ XB-C18 column (250 mm × 4.6 mm, 5 μm) with 75% methanol-water as the mobile phase separation, fluorescence detector detection. Results Welchrom ~ P-SCX strong cation exchange column pretreatment of pepper products purification with better impurity removal, more stability, better reproducibility of the method and other advantages, and therefore Welchrom ~ P-SCX small Column of pepper products pretreatment purification. Rhodamine B had a good linearity (r ~ 2> 0.9995) in the range of 1.0 ~ 100.0μg / L, the recoveries of two pepper products ranged from 91.4% to 106.5%, and the relative standard deviations (RSDs) ranged from 2.1% to 4.3% between. Conclusion The sensitivity, accuracy and precision of this method are in accordance with the detection requirements of rhodamine B, and it is simple and rapid. It is suitable for the accurate determination of rhodamine B in pepper products.