高效液相色谱柱前衍生法测定水产品中的游离甘氨酸

Determination of Free Glycine in Aquatic Products by High Performance Liquid Chromatography Pre-column Derivatization

建立一种高效液相色谱柱前衍生法测定水产品中的游离甘氨酸。采用C18色谱柱,以乙腈+0.01 mol/L乙酸钠溶液(pH=4.2)(1.2.7)=3+7作为流动相,检测波长为254 nm,利用高效液相色谱法-二极管阵列器进行外标法定量测定。实验结果表明,甘氨酸方法检出限为50 mg/kg,在浓度为1~50μg/mL范围内成线性关系,回收率为90.4%~101%,相关标准偏差(RSD)为2.5%~3.3%。该方法方便,灵敏度高,定性定量准确,分析时间短,可很好地实现水产品类样品中游离甘氨酸的测定。同时此方法样品检测结果与氨基酸分析仪样品结果偏差均在10%范围内,也可作为氨基酸分析仪法外的补充方法。

A method was established pre-column derivatives for the determination of free glycine in aquatic products by high-performance liquid chromatography.The samples were derivatized by dansulfoyl chloride precolumn,and acetonitrile+0.01 mol/L sodium acetate solution(pH=4.2)(1.2.7)=3+7 was used as mobile phase for isocratic elution on C18chromatographic column,the detection wavelength was 254 nm,High performance liquid chromatography-diode array device was used for determination,and external standard method was used for quantification.The results showed that the detection limit of the glycine method was 50 mg/kg.The linear range was 1~50μg/mL with a good linear relationship.The recoveries were 90.4%-101%,and the correlation standard deviations(RSD)were 2.5%-3.3%.The method was convenient,high sensitivity,accurate qualitative and quantitative,short analysis time,and could be well realized for the determination of free glycine in aquatic product samples.At the same time,the deviation between the sample results of this method and the sample results of amino acid analyzer was within 10%.It could also be used as a supplementary method apart from the method of amino acid analyzer.