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固相萃取-高效液相色谱法测定黄酒中氨基甲酸乙酯
引用本文:诸葛庆,李博斌,江涛,寿谦,葛乐勇,曾红艳. 固相萃取-高效液相色谱法测定黄酒中氨基甲酸乙酯[J]. 酿酒科技, 2012, 0(1): 112-115
作者姓名:诸葛庆  李博斌  江涛  寿谦  葛乐勇  曾红艳
作者单位:国家黄酒产品质量监督检验中心,浙江绍兴,312071
基金项目:浙江省质量技术监督系统科技项目,浙江省黄酒技术产业与装备重点实验室项目
摘    要: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。

关 键 词:分析方法  高效液相色谱法  黄酒  氨基甲酸乙酯  固相萃取

Determination of Ethyl Carbamate in Yellow Rice Wine by Solid- phase Extraction Coupled with HPLC
ZHUGE Qing,LI Bobin,JIANG Tao,SHOU Qian,GE Leyong and ZENG hongyan. Determination of Ethyl Carbamate in Yellow Rice Wine by Solid- phase Extraction Coupled with HPLC[J]. Liquor-making Science & Technology, 2012, 0(1): 112-115
Authors:ZHUGE Qing  LI Bobin  JIANG Tao  SHOU Qian  GE Leyong  ZENG hongyan
Affiliation:(National Center for Quality Supervision & Testing of Rice Wine,Shaoxing,Zhejiang 312071,China)
Abstract: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.
Keywords:analytic methods  HPLC  yellow rice wine  ethyl carbamate  solid -phase extraction
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