摘要
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。
A high performance liquid chromatographic method with post-column photochemical derivation and fluorescence detection was developed for the analysis of thiamine in foods. A C18, column was used for separation, and elution was performed with a pH 4.0 phosphate buffer (0.1 mel/L) containing 2%acetonitrile. When the eluate was on-line converged with a mixed 0.75% Na2SO3-4% NaOH solution,thiamine in the eluate was transferred to an intensive fluorescence compound by post-column photochdemical derivation that occurred in a knotted polytetrafluoroethylene reator, and detectad by a spectrofluorimetor. Under optimized conditions, a detection limit of 3.8μg/L thiamine was achieved with the injection volume of 20μL, and a linear calibration curve was obtained in the range of 0.033 ~ 10 mg/L thiamine. RSD was in the level of 1.8%, and the recoveries of spiked analyte were in the range of 97% ~ 102%. The developed method was applied to determine the thiamine conents in pork liver and milk powder, and satisfactory results were obtained.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2000年第5期554-558,共5页
Chinese Journal of Analytical Chemistry
基金
浙江省分析测试基金
关键词
高效液相色谱法
荧光检测
维生素B1
食品
High performance liquid chromatography, photochemical derivatization, fluorescence detection, thiamine, foods