凝胶渗透色谱-气相色谱/串联质谱法分析辐照肉松与乳粉中2-十二烷基环丁酮含量

Determination of 2-dodecylcyclobutanone in irradiated dried meat floss and milk powder by gel permeation chromatography-gas chromatography-tandem mass spectrometry

中文关键词:  凝胶渗透色谱  气相色谱-串联质谱法  2-十二烷基环丁酮  辐照肉松  辐照乳粉

英文关键词:gel permeation chromatography  gas chromatography-tandem mass spectrometry  2-dodecylcyclobutanone  irradiated dried meat floss  irradiated milk powder

中文摘要:

      目的 利用凝胶渗透色谱-气相色谱/串联质谱法分析不同辐照剂量处理的肉松与乳粉中2-十二烷基环丁酮含量。方法 样品中目标组分经正己烷超声提取, 使用凝胶渗透色谱净化去除大分子成分并结合在线浓缩处理后, 利用气相色谱-串联质谱进行分析检测, 其中质谱扫描采用多反应监测模式(multi reaction monitoring mode, MRM), 所监测离子对为(m/z)98.1＞83.1、(m/z)98.1＞70.1、(m/z)98.1＞55.0、(m/z)112.2＞97.1。结果 在10~1000 μg/L范围内2-十二烷基环丁酮标准曲线方程具有良好的线性关系, 方法的检出限和定量限分别为2.3、7.7 μg/kg, 在20、100、500 μg/kg 3个水平下的平均加标回收率在73.5%~98.2%之间, 相对标准偏差小于6.2%。结论 该方法灵敏度高、准确性好、操作简单, 可用于辐照肉松与乳粉中2-十二烷基环丁酮检测。

英文摘要:

      Objective To analyze the content of 2-dodecyl cyclobutanone in meat floss and milk powder treated with different irradiation doses by gel permeation chromatography-gas chromatography/tandem mass spectrometry. Methods The target components were extracted by N-hexane ultrasound, purified by gel permeation chromatography to remove macromolecular components and concentrated on-line, and then analyzed by gas chromatography-tandem mass spectrometry. The mass spectrometry scanning adopted multi-reaction monitoring mode (MRM), and the monitored ion pairs were (m/z) 98.1>83.1, (m/z) 98.1>70.1, (m/z) 98.1>55.0, (m/z) 112.2>97.1. Results The standard curve equation of 2-dodecyl cyclobutanone had a good linear relationship in the range of 10–1000 g/L. The detection limit and quantitative limit of the method were 2.3 g/kg and 7.7 g/kg, respectively. The average recoveries of 2-dodecyl cyclobutanone were 73.5%–98.2% and the relative standard deviations were less than 6.2% at the levels of 20, 100, 500 g/kg. Conclusion This method has high sensitivity, good accuracy and simple operation, and can be used for the detection of 2-dodecyl cyclobutanone in irradiated meat floss and milk powder.