高效液相色谱法测定酱卤肉中酸性橙Ⅱ的优化

Optimization of determination of acid orange Ⅱ in braised pork by high performance liquid chromatography

中文关键词:  酸性橙Ⅱ  高效液相色谱法  二极管阵列检测器  酱卤肉

英文关键词:acid orange Ⅱ  high performance liquid chromatography  diode array detector  braised pork

中文摘要:

      目的 建立高效液相色谱法测定酱卤肉中酸性橙Ⅱ的检测方法。方法 样品经氨水甲醇提取液提取, 调节pH沉淀蛋白后, 过混合弱阴离子(mixed weak anion, PWAX)固相萃取柱净化。采用20 mmol/L乙酸铵(A)和甲醇(B)作为流动相进行等度洗脱, 采用二极管阵列检测器(diode array detector, DAD)对酸性橙Ⅱ进行多波长检测。结果 本方法可在10 min内完成目标化合物与杂质的分离。酸性橙Ⅱ在0.1、0.5和2.0 mg/kg添加水平的回收率提升至76.0%~92.5%, 相对标准偏差小于15%(n=6), 方法检出限为0.1 mg/kg。结论 该方法快速、准确、灵敏, 适合酱卤肉等蛋白质含量高的样品中酸性橙Ⅱ的大批量检测。

英文摘要:

      Objective To establish a method for the determination of acid orange Ⅱ in marinated pork by high performance liquid chromatography. Methods The sample was extracted with ammonia methanol extract, adjusted pH to precipitate protein, and purified by mixed weak anion (PWAX) solid phase extraction column. Using 20 mmol/L ammonium acetate (A) and methanol (B) as mobile phases for isocratic elution, diode array detector (DAD) was used for multi-wavelength detection of acid orange II. Results This method completed the separation of the target compound and impurities within 10 minutes. The recoveries were ranged from 76.0%?92.5% with 3 spiked levels of 0.1, 0.5 and 2.0 mg/kg. The relative standard deviations (RSDs) were less than 15% (n=6), and the limits of detection was 0.1 mg/kg. Conclusion This method is fast, accurate and sensitive, and is suitable for the mass detection of acid orange II in samples with high protein content such as braised pork.