固相萃取-高效液相色谱-荧光法测定辣椒制品中罗丹明B
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, 5 μm)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1.0~100.0 μg/L范围具有良好的线性(r2＞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 the rhodamine B (RB) in pepper products by solid phase extraction–high performance liquid chromatography-fluorescence detector (SPE-HPLC-FLD). Methods The sample were extracted by acetonitrile and 20% acetone-n-hexane solution, then purified and concentrated with a strong positive ion exchange SPE column (Welchrom? P-SCX) and a neutral alumina SPE column (Welchrom? Alumina). The HPLC separation was performed on a Welch Ultimate? XB-C18 HPLC column (250 mm × 4.6 mm , 5 μm), eluted with a mobile phase consisting of methanol and water (75:25, V:V). The analyzed sample was detected by fluorescence detector. The content of RB in pepper products was measured using peak area external standard method. Results The results showed that the method of using Welchrom? P-SCX SPE column to pre-treat sample had higher efficiency, stability and better repeatability. The calibration curve showed a good linearity in the range of 1.0~100.0 μg/L with correlation coefficient (r2) greater than 0.9995. The recoveries were 91.4%~106.5% at three spiked levels with the relative standard deviations (RSDs) of 2.1%~4.3%. Conclusion This method is sensitive, accurate and precise, which is very in accordance with technical standards of the RB detection. It is suitable for routine detection of the RB in pepper products.
标题：固相萃取-高效液相色谱-荧光法测定辣椒制品中罗丹明B
英文标题：Determination of rhodamine B in pepper products by solid phase extraction–high performance liquid chromatography-fluorescence detector
作者：
薛昆鹏 浙江师范大学物理化学研究所
金小青 浙江师范大学物理化学研究所
余冲 浙江月旭材料科技有限公司
赵岳星 浙江师范大学物理化学研究所
中文关键词:固相萃取,高效液相色谱-荧光检测法,辣椒制品,罗丹明B,
英文关键词:solid phase extraction,high performance liquid chromatography-fluorescence detector,pepper products,rhodamine B,
发表日期：2016-05-16
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