摘要
目的:用凝胶色谱净化液相色谱-荧光法测定天然维生素E中苯并芘残留量含量。方法:采用不同比例的乙酸乙酯∶环己烷溶解样品、GPC净化、C18柱分离,进行荧光检测;以苯并芘溶解性确定GPC流动相,确定GPC的收集时间段,测试油脂净化能力。结果:随着乙酸乙酯比例的增加,苯并芘溶解性更好,选择乙酸乙酯∶环己烷(1∶1,V/V)为流动相;苯并芘的流出时间段集中在18~24 min,为保证低含量水平的测定结果准确性,将GPC收集时间段定为17~25 min;在0. 1~20. 0μg/L的浓度范围内,色谱峰面积与其浓度之间线性关系良好,相关系数为0. 999,检测限(S/N=3)为0. 02μg/kg,定量限(S/N=10)为0. 05μg/kg;在0. 05、0. 10、0. 20及2. 00μg/kg添加浓度水平上的平均回收率为98. 0%、93. 3%、96. 4%及98. 0%,相对标准偏差(RSD)分别为3. 8%、2. 6%、3. 6%及2. 1%。结论:成功建立天然维生素E中苯并芘残留量测定的GPC净化高效液相色谱法。
Objective:To determine the volume of benzopyrene residues in natural vitamin E by gel permeation chromatography(GPC)combined with high-performance liquid chromatography.Methods:The dissolved samples of ethyl acetate and hexane with different proportion were adopted;GPC purification and C18 column separation were applied and fluorescence detection was conducted.The solubility of Benzopyrene was used to determine the GPC mobile phase and collection time,and detect its oil purification capacity.Results:With the increase of proportion,Benzopyrene was more soluble.The 1∶1 proportion of ethyl acetate and hexane was selected as the mobile phase.The outflow time of Benzopyrene was concentrated to 18~24 min,For the sake of accuracy,the outflow time was established as 18~24 min.In the concentration range of 0.1~20.0μg/L,there was a good linear relationship between chromatographic peak area and the concentration with a correlation coefficient of 0.999,the detection limit(S/N=3)as 0.02μg/kg,and the quantitative limit(S/N=10)as 0.05μg/kg.The average recovery rates was 98.0%,93.3%,96.4%and 98.0%in the added concentration level of 0.05,0.10,0.20 and 2.00μg/kg.The relative standard deviation(RSD)was 3.8%,2.6%,3.6%and 3.8%,respectively.Conclusion:Our method of GPC purification and high-performance liquid chromatography is successful in the determination of the volume of benzopyrene residues in natural vitamin E.
作者
田广
刘敏
苏艳丽
TIAN Guang;LIU Min;SU Yanli(Guihang Guiyang Hospital,Guiyang 553009,China;Guiyang Nursing Vocational College,Guiyang 550081,China)
出处
《贵州医科大学学报》
CAS
2020年第6期684-688,共5页
Journal of Guizhou Medical University
关键词
色谱法
高效液相
维生素E
苯并芘
残留量
chromatography
high pressure liquid
vitamin E
benzo(a)pyrene
residues
