固相萃取-高效液相色谱法测定黄酒中氨基甲酸乙酯

建立一种反相高效液相色谱法测定黄酒中氨基甲酸乙酯的方法。样品经固相萃取柱净化后衍生，采用反相C18色谱柱XB—Cfsf4．6mm×250mm,5μm），以乙腈-0．02moL／L乙酸纳水溶液为流动相进行梯度洗脱，流速为lmL／min；设定荧光检测器中激发波长为233nm，发射波长为600nm，对黄酒中的氨基甲酸乙酯进行检测。结果表明，在50．0-250．0μg／L添加量范围内，平均回收率为92．9％，相对标准偏差为4．5％（n=6）。方法的检出限为10μg／L，线性范围为100～1500μg／L（R=0．9995），测定结果与标准气相色谱一质谱法基本相同。所建立的方法可以作为黄酒中氨基甲酸乙酯的检测方法。

Determination of Ethyl Carbamate in Yellow Rice Wine by Solid- phase Extraction Coupled with HPLC

A reverse phase HPLC method for the determination of ethyl carbamate in yellow rice wine had been developed.Wine samples were firstly pretreated by solid-phase extraction,ethyl carbamate was separated on a XB-C18(4.6mm×250 mm,5 μm) by using gradient elution(acetonitrile and 0.02 moL/L sodium acetate as the mobile phase) at a flow rate of 1mL/min and detected by a fluorescence detector(λex=233 nm,λem=600 nm).At the spike levels of 50.0,100.0 and 250.0 μg/L,the average recovery for ethyl carbamate was 92.9% with RSD as 4.5 %(n = 6),the detection limit was 10 μg/ L,and the linear range was from 100～1500 μg/L(R=0.9995.The determination results by this method were almost the same as those by GCMS.Therefore,this method could be use to determine ethyl carbamate in yellow rice wine.