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

Determination of free gossypol in edible vegetable oil using ultra performance liquid chromacography with tandem mass spectrometry

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

中文摘要:

      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。

英文摘要:

      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.