高效液相色谱法同时测定秋葵干蔬中的脂溶性维生素A、E、K_3

Simultaneous Determination of Fat-soluble Vitamins A,E and K_3 in Dried Okra by High Performance Liquid Chromatography

建立了同时测定秋葵干蔬中脂溶性维生素A、E、K3的反相高效液相色谱法。样品皂化后,采用C18色谱柱(150 mm×4.6 mm,5μm i.d.)进行分离,以甲醇为流动相,流速1.0 mL/min,二极管阵列检测器(DAD)在325、290、244 nm波长下同时检测,外标法定量。结果表明,脂溶性维生素A、E、K3在0.1～20.0 mg/L范围内呈良好线性,相关系数均大于0.99;3种脂溶性维生素的回收率为88%～95%,相对标准偏差(RSD)为0.8%～3.9%;检出限(LODs,S/N=3)分别为0.3、0.6、0.1 mg/kg,定量下限(LOQs,S/N=10)分别为1.0、2.0、0.3 mg/kg。该方法具有较高的准确度和精密度,能够满足实际检测的需要。

A method was developed for the simultaneous determination of fat-soluble vitamin A,E and K3 in dried okra by reversed phase high performance liquid chromatography coupled with diode array detection.The sample was first extracted with ethanol and followed by saponification with 50% KOH solution,then extracted with petroleum ether.The extract was separated on an Agilent Eclipse XDB C18 column（150 mm× 4.6 mm,5 μm i.d.） at 30 ℃,using methanol as mobile phase at a flow rate of 1.0 mL/min.The target compounds were simultaneously detected at 325,290,244 nm,respectively,and quantified by the external standard method.The results showed that the linear ranges for fat-soluble vitamins A,E,K3 were in the range of 0.1-20.0 mg/L with correlation coefficients more than 0.99.The spiked recoveries of three fat-soluble vitamins from dry okra sample were in the range of 88%-95% with RSDs of 0.8%-3.9%.The limits of detection（LODs,S/N=3） of VA,VE and VK3 were 0.3,0.6,0.1 mg/kg,respectively,and the limits of quantitation（LOQs,S/N=10） were 1.0,2.0,0.3 mg/kg,respectively.The developed method was simple and accurate,and could meet the demands for actual detection.