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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/串联质谱测定方法。方法:植物油样品经无水乙醇提取后用热水溶解,正己烷脱脂后,过Oasis HLB固相萃取小柱,采用Extend C18柱(250 mm×4.6 mm i.d.,5μm),以水+甲醇(65+35,v/v)为流动相进行分离,紫外检测波长为219 nm,同时在电喷雾电离(ESI)正离子模式下采用多反应监测(MRM)模式进行检测,定量离子对为m/z 165→138。结果:蓖麻碱在紫外检测条件下,在50.0~10000.0μg/kg范围内呈良好线性关系,回收率在92.7%~97.8%范围,日间RSD小于5.4%,检出限为50.0μg/kg。在串联质谱检测条件下,在0.5~50.0μg/kg范围内呈良好线性关系,回收率在90.0%~96.5%范围,日间RSD小于10.5%,检出限为0.5μg/kg。结论:本方法简便、灵敏、重现性好,能满足食用植物油中微量蓖麻碱的定量检测要求。
Objective: To establish a method for the determination of trace ricinine in edible vegetable oil by high performance liquid chromatography with UV / tandem mass spectrometry. Methods: The vegetable oil samples were extracted with absolute ethanol and then dissolved in hot water. After the n-hexane was degreased, the samples were run on an Oasis HLB solid-phase extraction cartridge. The samples were eluted with an Extend C18 column (250 mm × 4.6 mm id, + 35, v / v) as the mobile phase. The UV detection wavelength was 219 nm. At the same time, it was detected by multi-reaction monitoring (MRM) mode in electrospray ionization (ESI) 165 → 138. Results: Under the UV detection conditions, ricinine showed a good linear relationship in the range of 50.0 ~ 10000.0μg / kg, the recovery was in the range of 92.7% ~ 97.8%, the intraday RSD was less than 5.4% and the detection limit was 50.0μg / kg . Under the condition of tandem mass spectrometry, the linearity was within the range of 0.5-50.0μg / kg, the recovery was in the range of 90.0% -96.5%, the intraday RSD was less than 10.5% and the detection limit was 0.5μg / kg. Conclusion: The method is simple, sensitive, reproducible, and can meet the quantitative detection requirements of trace ricinine in edible vegetable oil.