摘要
目的:建立柱前衍生-反相高效液相色谱同时测定蜂王幼虫冻干粉中16种氨基酸含量的方法,并测定29批蜂王幼虫冻干粉中水解氨基酸含量。方法:以异硫氰酸苯酯为柱前衍生试剂,采用Waters Symmetry C18色谱柱(4.6 mm×250 mm,5μm)分析,以乙腈-水(4∶1)溶液和0.03 mmol/L醋酸钠-乙腈(355-15,ph=6.5)进行梯度洗脱,流速1.0 mL/min,在254 nm波长处测定氨基酸含量。结果:氨基酸在0.0625~1.2500 mmol/L范围内具有良好的线性关系(r≥0.9974),平均平均回收率在94.97%~99.50%之间;检出限为0.0005~0.0015 mmol/L,定量限为0.0075~0.0240 mmol/L。结论:该方法简便易行、准确性高、稳定性好,适于蜂王幼虫冻干粉中氨基酸定量检测。
Objective：To establish a method for the determination of 16 amino acids in frozen dry powder of queen bee larva using precolumn derivatization and reversed-phase high performance liquid chromatography,and to determine the content of amino acid in 29 batch of queen bee larva freeze dried powder.Methods ：Precolumn derivatized with phenylisothiocyanate（PITC）combined with Waters Symmetry C18 chromatography column（4.6 mm×250 mm,5μm）were used;gradient elution was performed with acetonitrile-water（4：1）solution and 0.03 mmol/L sodium acetate-acetonitrile（355-15,ph=6.5）;flow rate was 1.0 mL/min,wavelength was 254 nm.Results ：The calibration curves of 16 amino acids exhibited a good linear relationship over the range from 0.0625 to 1.2500 mmol/L.Mean recoveries for amino acids and biogenic amines were between 94.97% and 99.50%.The limits of detection（LODs）for 16 free amino acids were in the range of 0.0005~0.0015 mmol/L,and the limits of quantification（LOQs）were 0.0075~0.0240 mmol/L.Conclusion：The method is simple,convenient,accurate and stable.It is suitable for the quantitative detection of amino acid in freeze-dried powder of queen bee larvae.
出处
《中国食品添加剂》
北大核心
2017年第11期176-182,共7页
China Food Additives
关键词
蜂王幼虫冻干粉
氨基酸
柱前衍生
反相高效液相色谱法
frozen dry powder of queen bee larva
amino acids
pre column derivatization
reversed-phase high performance liquid chromatography（RP-HPLC）
