在线净化二维液相色谱快速检测食品中维生素A、D、E

目的 利用三泵两阀二维液相色谱系统,建立食品中维生素A、D、E在线二维液相色谱快速检测方法。方法 采用中心切割方法搭建在线二维液相色谱分离系统,以高聚合物为填料的具有耐强碱溶液能力的PLRP-S色谱柱作为净化样品皂化液的固相萃叐(solid phase extraction,SPE)柱,以C_18为一维色谱柱分离维生素A和E,以多环芳烃(polycyclic aromatic hydrocarbon, PAH)色谱柱为二维色谱柱分离维生素D2和D3。一维色谱确立维生素D的切割时间,由C_18小柱捕获维生素D,建立在线二维液相色谱分析方法。利用样品和标品液对建立的方法进行方法学验证,同时比较该方法与GB 5009.82-2016对实际样品的测试结果。结果 维生素A、D、E在试验标准曲线范围内线性系数r>0.999,定量限分别为30μg/100g, 2μg/100 g和120μg/100 g,与国标一致;该方法 3水平加标回收率为90.4%～101.7%,可以满足目前食品中维生素A、D、E的检测需求。结论本文建立的测试方法操作简单高效、自动化程度高、准确度高、重复性好,适合于大批量样品的测试。

Rapid detection of vitamin A,D and E in food by on-line purification two-dimensional high performance liquid chromatography

Objective To establish an on-line two-dimensional liquid chromatographic method for the determination of vitamins A, D and E in food by using a three-pump and two-valve two-dimensional liquid chromatographic system. Methods An on-line two-dimensional liquid chromatography separation system was set up by central cutting method. The PLRP-S column with high polymer as filler which had strong alkali resistance was used as the solid phase extraction(SPE) column for purifying saponification solution of samples. Vitamin A and E were separated by C18 as one-dimensional column, and vitamin D2 and D3 were separated by polycyclic aromatic hydrocarbon(PAH) as two-dimensional column. One-dimensional chromatography confirmed the cutting time of vitamin D, VD was captured by C18 column, and then established on-line two-dimensional liquid chromatography analysis method. Samples and standard solutions were used to conduct the validation of the establishe d method, and the test results of actual samples were compared by using established method and GB 5009.82-2016. Results The linear coefficients of vitamin A, D and E were all more than 0.999 in the range of standard curves. The limits of quantitation were 30 μ g/100 g, 2 μ g/100 g and 120 μ g/100 g, which were consistent with the national standard GB5009.82-2016. The recoveries of vitamin A, D and E at 3 levels of this method were all between 90.4% and 101.7%,which could meet the detection requirements of vitamin A, D and E in food. Conclusion The method is simple,efficient, highly automated, accurate and reproducible, which is suitable for the determination of large quantities of samples.