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    反相高效液相色谱法测定油脂中抗氧化剂特丁基对苯二酚

    RP-HPLC DETERMINATION OF ANTIOXIDANT t-BUTYL HYDROQUINONE IN FAT AND OIL

    • 摘要: 采用反相高效液相色谱法分离并测定了加入于油脂中的抗氧化剂t-丁基对苯二酚(t-BHQ).适量的油脂试样溶于n-已烷中,其中的t-BHQ用甲醇萃取.含有t-BHQ的甲醇溶液进样至仪器中进行分离和测定.采用Symmetry Shield RP-C18作固定相;流动相系由甲醇及0.001 mol·L-1磷酸按60比40的体积比混合配成,并用0.001 mol·L-1乙酸及0.001 mol·L-1磷酸组成的缓冲控制流动相的酸度至pH 5.0.t-BHQ浓度在0.010 07-0.402 8 g·L-1范围内与所测主峰面积之间呈线性关系.方法的检出限(S/N=2)为0.020 14 μg.无论日间或日内测定的保留时间值或峰面积值,计算所得的RSD值均小于3.4%,说明仪器的重复性和稳定性良好.回收试验的结果表明测定的回收率在91.8%-94.0%之间,一次分析仅需6 min.

       

      Abstract: RP-HPLC was applied to the determination of t-butylhydroquinone (t-BHQ),which is added to food-stuffs as antioxidant.An appropriate quantity of sample was dissolved in n-hexane,and its t-BHQ was extracted with methanol.which was introduced into the HPLC instrument for separation and determination.The symmetry shield RP C18 was used as stationary phase,and a mixed solution containing CH3OH and 0.001 mol·L-1 H3PO4 in the ratio of 60 to 40 by volume (pH 5.0) was used as the mobile phase.UV detection at wavelength of 280 nm was adopted.Buffer solution prepared from 0.001 mol·L-1 HOAc and 0.001 mol·L-1 H3PO4 was used to control the acidity of the mobile phase.Linear relationship between peak area and concentration of t-BHQ was obtained in the range of 0.010 07-0.402 8 g·L-1,and the detection limit (S/N=2) was found to be 0.020 14 μg.In the test for precision,the RSDs obtained in the between-day and within-day measurement of retention time or of peak area were all less than 3.4%.Recoveries in the range from 91.8% to 94.0% were found in the test for recovery.Only 6 min were required for a whole analysis.

       

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