柱前衍生高效液相色谱法测定贝类产品中氨基酸含量

采用柱前衍生高效液相色谱法,测定了3种贝类中天冬氨酸、赖氨酸、亮氨酸等17种氨基酸含量。衍生试剂为6-氨基喹啉基-N-羟基琥珀酰亚胺基甲酸酯(AQC),流动相为醋酸盐-磷酸盐缓冲溶液、乙睛、水,梯度洗脱。色谱柱为AccQ·Tag(Waters)氨基酸分析柱,紫外检测。结果显示,氨基酸浓度与峰面积呈良好的线性关系,线性范围10～80μmol/L,检出限为0.23μmol/L,相关系数均在0.998以上,相对标准偏差RSD在2.1%～4.8%之间,回收率在91.3%～113.2%之间。

Determination of Amino Acids in Shellfish Samples by High Performance Liquid Chromatography with Precolumn Derivatization

The technology of precolumn derivatization, along with high performance liquid chromatography gradient elution method was used in determining contents of amino acids in shellfish products. A high-efficiency AccQ·Tag(Waters) column, acetate-phosphate buffer, acetonitrile, and twice distilled water were prepared in gradient elution. AQC(6-aminoquinoly-N- hydroxysuccinimidy carbamate), a derivation reagent, was used for sample derivatization. Conditions of the test were: column temperature 37℃, wavelength 248nm and flow rate 1.0ml/min.The results showed that concentration of amino acids and peak areas achieve a nice linear relations (r is higher than 0.998) with linear range 10～80μmol/L. RSD is of 2.1%～4.8%. The limit of detection is 0.23μmol/L. The ranges of recovery of amino acids are from 91.3%～113.2%.