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目的:建立食用植物油中微量蓖麻碱的高效液相色谱、紫外光谱和离子阱质谱的定性鉴别体系。方法:植物油样品经无水乙醇提取,热水溶解,正己烷脱脂后,经Oasis HLB固相萃取小柱净化,采用Extend C18柱(250 mm×4.6 mmi.d.,5μm),以水+甲醇(65+35,v/v)为流动相进行色谱分离后,采用二极管阵列检测器(DAD)在线检测,利用与标准品对照、紫外光谱在线扫描和三维光谱图谱等进行初筛;采用电喷雾电离离子阱质谱(ESI-IT-MS)研究其质谱行为,特别是碱金属加合离子特征和二级质谱裂解特征,进行确证鉴别。结果:DAD在线扫描提供了丰富的蓖麻碱光谱信息,高效液相色谱结合DAD在线扫描光谱、色谱保留时间及三维光谱图能进行较准确的初步定性;蓖麻碱在电喷雾正离子模式下具有明显的碱金属阳离子加合倾向,如锂、钠、钾等的特征加合离子;其分子离子峰经串联质谱裂解产生有特征的碎片离子,这些碎片离子可作为定性鉴别的确证依据。结论:本方法建立的高效液相色谱、紫外光谱及串联质谱的联合定性方法适用于植物油中微量蓖麻碱的掺伪、掺假和中毒应急检测的筛选和确证检测。
Objective: To establish a qualitative identification system of trace ricinine in edible vegetable oil by high performance liquid chromatography, ultraviolet spectrum and ion trap mass spectrometry. Methods: The samples of vegetable oil were extracted with absolute ethanol, dissolved in hot water, defatted with hexane and cleaned up with Oasis HLB solid phase extraction cartridges. The samples were extracted on an Extend C18 column (250 mm × 4.6 mm id, 5 μm) (65 + 35, v / v) as the mobile phase, and then detected by diode array detector (DAD) on-line, and compared with standard samples, UV online scanning and three- Ionization ion trap mass spectrometry (ESI-IT-MS) to study its mass spectrometry behavior, especially the characteristics of alkali metal ions and secondary mass spectrometry lysis characteristics, to confirm the identification. Results: DAD online scanning provided abundant information of ricinine spectrum. High performance liquid chromatography combined with DAD on-line scanning spectroscopy, chromatographic retention time and three-dimensional spectroscopy can be used to conduct more accurate preliminary qualitative analysis. In the electrospray positive ion mode It has the obvious adduct tendency of alkali metal cation, such as lithium ion, lithium ion, sodium ion, potassium ion and so on. The molecular ions are cleaved by tandem mass spectrometry to produce characteristic fragment ions. These fragment ions can be used as confirmation basis for qualitative identification. CONCLUSION: The method of HPLC, UV and tandem mass spectrometry established by this method is suitable for screening and confirmatory detection of adulteration, adulteration and poisoning emergency detection of trace ricinine in vegetable oil.