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研究柱后光化学衍生荧光检测高效液相色谱分离测定食品中维生素B1的方法。采用C18柱,以含有2%乙腈的pH4.0磷酸盐缓冲液(0.1mol/L)作流动相反相分离,猪肝等食品中的维生素B1可与其它杂质达到完全分离。色谱流出液在柱后与0.75%Na2SO3-4%NaOH的混合试剂溶液在线汇合后流经一聚四氟乙烯(PTFE)细管制成的光化学反应器时,维生素B1转化为强荧光产物,由荧光检测器测定。在最佳条件下,进样20μL检测限为3.8μg/L,工作曲线的线性范围为0.033-10mg/L,相对标准偏差(RSD)为1.8%,标准加入回收率为97%-102%。所建立的方法用于鲜猪肝和奶粉中维生素B1的测定,取得了满意的结果。
Study on post-column photochemical derivatization fluorescence detection of high-performance liquid chromatography for the determination of vitamin B1 in foods. Using a C18 column, the mobile phase was separated by reversed-phase mobile phase at pH 4.0 phosphate buffer (0.1 mol / L) containing 2% acetonitrile. Vitamin B1 in pork and other foods was completely separated from other impurities. The chromatographic effluent is converted to a strong fluorescent product when it is passed through a photochemical reactor made of a polytetrafluoroethylene (PTFE) thin tube after online confluence of a mixed reagent solution of 0.75% Na2SO3-4% NaOH and a column, Measured by fluorescence detector. Under the best conditions, the limit of detection of 20μL injection was 3.8μg / L, the linear range of the working curve was 0.033-10mg / L, the relative standard deviation (RSD) was 1.8% and the standard addition recovery was 97 % -102%. The established method was applied to the determination of vitamin B1 in fresh pig liver and milk powder, and satisfactory results were obtained.