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目的建立保健食品中维生素D3的固相萃取-超高效液相色谱方法。方法样品经皂化、萃取、定容后,利用硅胶柱固相萃取的净化技术,采用C18柱分离,甲醇水混合溶液作为流动相,PDA检测器检测,检测波长为264 nm。结果经硅胶固相萃取柱净化后,杂质能较好的去除,维生素D3的浓度为0.1μg/ml~5.0μg/ml时,其峰面积与质量浓度呈良好的线性关系回归方程为y=46 152x-1 735.1,相关系数(r)为0.999 6,回收率为87.8%~105.8%,相对标准偏差(RSD)为1.28%~3.58%(n=6),方法的检出限为1.0μg/100 g。结论利用本方法,可以测定保健食品中维生素D3含量,经净化后可消除杂峰的干扰且峰形较好,回收率高、快速简便,是测定保健食品中维生素D3含量的有效定量方法。
Objective To establish a method for the determination of vitamin D3 in health foods by solid-phase extraction-ultra performance liquid chromatography. Methods After saponification, extraction and determination, the samples were separated on a C18 column with methanol-water mixed solution as the mobile phase and detected by a PDA detector at a detection wavelength of 264 nm using silica gel column solid-phase extraction. Results After silica gel SPE purification, the impurities could be removed well. The linear regression equation was y = 46 when the concentration of vitamin D3 was 0.1μg / ml ~ 5.0μg / ml The relative standard deviations (RSDs) were 1.28% ~ 3.58% (n = 6). The detection limit of this method was 1.0μg / 100 g. Conclusion This method can be used to determine the content of vitamin D3 in health food. After being purified, it can eliminate the interference of impurity peak and has a good peak shape, high recovery and quickness and convenience. It is an effective and quantitative method for the determination of vitamin D3 in health food.