摘要
目的:建立反相高效液相色谱-二极管阵列检测法(HPLC-DAD)同时测定食品中维生素A、维生素D和维生素E(α-生育酚)的含量.方法: 取一定量食品样品加入乙醇、氢氧化钾及焦性没食子酸,80℃水浴皂化 30 min,石油醚提取后,氮气吹扫浓缩致干后用流动相溶解,进样 10 μl 分析;色谱条件为:色谱柱Supelco C18柱(15 cm×4.6 mm,5 μm),流动相甲醇∶水(93:7),柱温 40℃,DAD扫描波长范围 190~370 nm,检测波长 325 nm(Vitamin A)、265 nm(Vitamin D)、294 nm(Vitamin E).结果:维生素A在 1.0~100.0 μg/L 浓度范围内线性良好,相关系数 r =0.9999;维生素D2在 1.0~100.0 μg/L 浓度范围内相关系数 r =0.9997;维生素D3在 1.0~100.0 μg/L 浓度范围内相关系数 r =0.9998;维生素E在 0.50~50.0 mg/L 浓度范围内相关系数 r =0.9999.维生素A、维生素D和维生素E的平均回收率基本在 95% 以上,用本法调查了119种食品中维生素A、维生素D和维生素E的含量.结论: 方法快速、灵敏、准确,样品处理简便易行,可用于食品中脂溶性维生素A、D、E的同时测定.
Objective: To determinate the concentrations of retinal, vitamin D and α-tocopherol in food using HPLC with diode array detector. Methods: Food samples were added in anhydrous alcohol, potassium hydroxide and pyro - gallic acid. The mixture was shaken and saponified at 80℃ for 30 minutes. The lipo - soluble vitamins were extracted by petroleum ether. The organic layer was dried by gas of N2, dissolved by mobile phase, and analyzed by HPLC. The HPLC system consisted of Suplco C18 column ( 15 cm×4. 6 mm,5 μm), mobile phase of methanol: water (93: 7), column temperature 40℃, wavelength of scan from 190 nm to 370 nm, DAD detector at 325 nm of retinal, 265 nm of vitamin D and 294 nm of α - tocopherol. Results: The linear ranges of determination of retinal, vitamin D2, vitamin Ds and α - tocopherol were 1.0 - 100.0μg/L( r = 0. 9999), 1.0 - 100. 0μg/L(r =0. 9997) ,1.0 - 100.0 μg/L(r =0. 9998) and 0. 50 -50.0 mg/L(r =0. 9999), respectively. The average rates of recovery of these vitamins were above 95%. 119 foods were collected, and retinal, vitamin D , α -tocopherol level were determined by this method. Conclusion: The method is sensitive, simply, rapid and accurate. It can be used to simultaneously determine liposoluble vitamins in food.
出处
《中国卫生检验杂志》
CAS
2005年第9期1047-1049,共3页
Chinese Journal of Health Laboratory Technology