水产品中5种磷脂含量的HPLC-ELSD检测分析

Determination and Analysis for Contents of Five Phospholipids in Aquatic Products by HPLC-ELSD Method

本研究建立了水产品中5种磷脂的高效液相色谱-蒸发光散射检测器(HPLC-ELSD)方法并测定了几种水产品及水产品性腺组织中5种磷脂的含量。采用氯仿-甲醇(2∶1,V/V)进行磷脂的提取,氨基固相萃取柱净化富集,HPLC-ELSD对牡蛎(Ostrea gigas tnunb)、虹鳟(Oncorhynchus mykiss)、刺参(Apostichopus japonicas)、磷虾(Euphausia)以及海胆(Echinoidea)黄、大闸蟹(Eriocheir sinensis)蟹黄、鲟鱼(Acipenser sinensis)子酱、刺参性腺中的磷脂组成和含量进行分析,该方法加标回收率为77%~102%,相对标准偏差为0.75%~9.78%,具有较好的回收率和良好的精密度。结果显示,上述样品中含量最高的磷脂均为磷脂酰胆碱,其中磷虾粉中磷脂酰胆碱含量最高为29.71~35.30 mg/g。磷脂酰乙醇胺除鲟鱼子酱样品外均有检出,其中刺参和牡蛎冻干粉样品中磷脂酰乙醇胺含量较高,含量范围分别为2.90~3.69 mg/g和2.49~4.40 mg/g,磷脂酰肌醇、溶血磷脂酰胆碱和鞘磷脂3种磷脂仅有少数品种有检出,且含量较低。综上,HPLC-ELSD法可以实现对鱼、贝、虾等水产品中5种磷脂组分的快速准确分析及定量,为水产品营养品质评价提供参考。

In this study,a high performance liquid chromatography-evaporative light scattering detector(HPLC-ELSD)method for 5 kinds of phospholipids in aquatic products was established,and then their contents in several aquatic products and gonadal tissues were determined.The mixture solution of chloroform and methanol(2∶1,v/v)was used to extract phospholipids,and amino solid-phase extraction column was applied to purify and enrich.The composition and content of phospholipids in Ostrea gigas tnunb,Oncorhynchus mykiss,Apostichopus japonicas,Euphausia,Echinoidea,crab spawn of Eriocheir sinensis and caviar of Acipenser sinensis were analyzed by HPLC-ELSD.The recoveries of this method were in ranges of 77%-102%with relative standard deviation(RSD)of 0.75%-9.78%,indicating that the method had good recoveries and satisfactory precision.The highest content of phospholipid in these aquatic products was phosphatidylcholines,among which the highest content of phosphatidylcholines in krill meal ranged from 29.71 mg/g to 35.30 mg/g.Phosphatidylethanolamine was detected in all above samples except sturgeon caviar,and the contents of phosphatidylethanolamine in the freeze-dried powder samples of stichopus japonicus and oyster were higher with content ranges of 2.90-3.69 mg/g and 2.49-4.40 mg/g.Phosphatidylinositol,lysophosphatidylcholine and sphingomyelin were only detected in a few varieties with low contents.In conclusion,the HPLC-ELSD method could realize the rapid and accurate analysis and quantification for five kinds of phospholipid components in fish,shellfish,shrimp and other aquatic products to provide a reference for the nutritional quality evaluation of aquatic products.