柱前DCI衍生-固相萃取-高效液相色谱法快速测定干酪中的6种生物胺

Using pre-column DCI derivatization,solid phase extraction and HPLC technique to detect quickly of biogenic amines in cheese

研究了利用RP—HPLC对干酪中6种生物胺进行测定，分别采用三氯醋酸、高氯酸、盐酸、无水乙醇、无水甲醇作为提取溶剂对干酪样品中的生物胺进行提取，经丹磺酰氯（DCI）柱前衍生后，利用固相萃取装置萃取生物胺衍生产物，然后上机检测．采用乙腈一超纯水为流动相，梯度洗脱，流速1mL／min，利用荧光检测器进行检测。结果表明，采用浓度为0．1m01／L的盐酸作为干酪中生物胺的提取试剂比其他4种溶剂更为适宜；固相萃取步骤的引入对进一步富集，纯化衍生产物起到了重要作用；干酪中的6种生物胺在25min内被快速检出，6种生物胺的整体回收率较高，相对标准偏差（RSD）为1．7-~6．7％，最低检出限0．0037-0．0182mg／L。该方法是一种针对干酪中6种常见生物胺的快速高效的检测方法。

Using R.P-HPLC technique to detect of six types biogenic amines in cheese. Adhibition trichloroacetic acid（TCA）,perchloric acid,, hydrochloric acid, absolute ethylalcohol, absolute methanol extract respectively biogenic amines in cheese.After pre-column DCI derivatiza- tion, take advantage of SPE Vacuum Manifold to extract the ramification, then apply for HPLC. The mobile phase is acetonitrile-ultrapure water, gradient elute.The flow-rate is lmL/min.Fluorescence detector is applied.The experimental result indicate,the using of 0.1 mol/L HCL for extract the biogenic amines in cheese is a more suitable extraction way than the others. The procedure of SPE is benefit of improving the purity of ramification. The six types biogenic amines in cheese is detected in 25 rain,and the recovery rate of six type biogenic amines is rela- tively high, The relative standard deviation （RSD） is 1.7%-6.7%.The limit of detection is 0.0037-0.0182 mg/L.So this experimental method is a rapid, efficient detection way for the six types biogenic amines in cheese.