高效液相色谱法同时测定柠檬中柠檬苦素和诺米林含量

Determination of limonin and nomilin contents in lemon by high performance liquid chromatography

中文关键词:  高效液相色谱法  柠檬  柠檬苦素  诺米林

英文关键词:high performance liquid chromatography  lemon  limonin  nomilin

中文摘要:

      目的 建立高效液相色谱法同时测定柠檬中柠檬苦素和诺米林含量。方法 样品经乙酸乙酯超声波辅助提取, 高速离心机分离得到提取液, 提取液经无水硫酸钠脱水处理, 旋转蒸发仪减压浓缩、定容后待测。使用Shiseido CAPCELL PAK MG Ⅱ C18色谱柱(250 mm×4.6 mm, 5.0 μm), 以乙腈-0.10%磷酸水溶液(45:55, V:V) 为流动相; 流速: 0.70 mL/min; 进样量: 10 μL; 检测波长: 215 nm。结果 柠檬苦素和诺米林在0.50~1000.0 mg/L质量浓度范围内呈良好线性关系, 线性相关系数r≥0.9993, 检出限为0.25、0.34 mg/L, 定量限为0.70、0.95 mg/L。3个添加水平(100.0、200.0和500.0 mg/kg)下的加标回收率为82.60%~108.7%, 相对标准偏差为3.56%~5.22%。结论 该方法具有操作简单, 重复性和稳定性好等优点, 可准确测定柠檬汁和柠檬皮中诺米林和柠檬苦素的含量。

英文摘要:

      Objective To establish a method for determination of the content of limonin and nomilin in lemon by high performance liquid chromatography (HPLC). Methods Limonin and nomilin were extracted by ethyl acetate with ultrasound assistance, centrifuged at high speed and filtered, the extract was dehydrated with anhydrous sodium sulfate, concentrated by the evaporator, and detected after constant volume. The detecting conditions were as follows: separation column: Shiseido CAPCELL PAK MG Ⅱ(250 mm×4.6 mm , 5.0 μm), mobile phase: acetonitrile and 0.10% ate aqueous solution (45:55, V:V) , flow rate: 0.70 mL/min, injection volume: 10 μL, and PDA detector wavelength: 215 nm. Results The calibration curve was liner in the range of 0.50-1000.0 mg/L with the correlation coefficients of more than 0.9993. The limits of detection were 0.25 and 0.34 mg/L and the limits of quantitation were 0.70 and 0.95 mg/L for limonin and nomilin. The recoveries of 3 different spiked levels (100.0, 200.0 and 500.0 mg/kg) were 82.60%-108.7%, with the relative standard deviations of 3.56%-5.22%. Conclusion The method has the advantages of simple operation, good repeatability and stability, which can accurately determine the content of limonin and nomilin in lemon juice and lemon peel.