超高效液相色谱-串联质谱法测定 食用植物油中的游离棉酚
目的 建立超高效液相色谱-电喷雾串联质谱测定食用植物油中游离棉酚的方法。方法 样品采用无水乙醇溶液提取, C18色谱柱分离, 电喷雾串联四极杆质谱仪进行检测。结果 棉酚的质量浓度在0.001~1.0 μg/mL范围内具有良好的线性关系。食用植物油中的棉酚在5、50、250 μg/kg 3个添加水平下, 平均回收率为70.6%~94.4%, 相对标准偏差小于12.0%; 方法检出限LOD(S/N≥3) 为1 μg/kg, 定量限LOQ(S/N≥10)为5 μg/kg。结论 该方法快速简单, 结果准确, 重现性好, 适用于食用植物油中的游离棉酚含量的测定。
Objective A method for the free gossypol in edible vegetable oil was developed using ultra performance liquid chromatography-electrospray ionization triple-quadruple tandem mass spectrometry (UPLC-ESI-MS-MS). Methods The free gossypol residue in the test samples was extracted with ethanol solution. The gradient chromatographic separation was performed using a C18 column (100 mm×2.1 mm, 2.6 μm), and analyzed by UPLC-ESI-MS-MS. The mass spectrometer was operated in the negative ion mode using multiple reaction monitoring (MRM) for qualitative and quantitative analysis. Results The linear range was from 0.001~1.0 μg/mL. The average recoveries of the gossypol ranged from 70.6% to 94.4% (n=6) at the spiking levels of 5?250 μg/kg with the relative standard deviation less than 12.0%. The limit of detection (LOD, S/N≥3) was 1 μg/kg and the limit of quantification (LOQ, S/N≥10) were 5 μg/kg. Conclusion The method is suitable for the determination of gossypol in edible vegetable oil.
标题：超高效液相色谱-串联质谱法测定 食用植物油中的游离棉酚
英文标题：Determination of free gossypol in edible vegetable oil using ultra performance liquid chromacography with tandem mass spectrometry
作者：
吴敏 厦门出入境检验检疫局
连英杰 厦门出入境检验检疫局
林立毅 厦门出入境检验检疫局
徐敦明 厦门出入境检验检疫局
黄志强 湖南省检验检疫科学技术研究院
中文关键词:超高效液相色谱-串联质谱,游离棉酚,食用植物油,
英文关键词:ultra performance liquid chromatography- tandem mass spectrometry (UPLC-MS-MS),free gossypol,edible vegetable oil,
发表日期：2014-02-23
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