摘要
目的建立葡萄酒中氨基甲酸乙酯（EC）含量的高效液相色谱。荧光检测器（HPLC—FLD）测定方法。方法葡萄酒样品经9-羟基吨衍生后，采用高效液相色谱-荧光法测定，以AgilentTC—C18色谱柱（250mm×4．6mm×5μm）分离，乙腈-O．02mol／L乙酸钠溶液为流动相，梯度洗脱，荧光检测器的激发波长为233nm，发射波长为600nm，衍生化反应时间30min，外标法计算含量，并与GC-MS方法比较，评价HPLC-FLD方法可靠性。结果Ec在10～500灿g／L范围内呈良好的线性关系，平均加标回收率为93．7％～106．0％，相对标准偏差为1．4％～2．8％，定量限为15μg／L。HPLC—FLD和GC．MS两种方法对葡萄酒的EC含量测定结果无明显差异。结论HPLC—FLD适合于葡萄酒中EC含量的快速测定。
Objective To evaluate the method for determining ethyl carbamate （EC） in wine by HPLC-FLD. Methods Samples were derived and determined by HPLC with a fluorescence detector. Using a Agilent TC-C18（250 mm ×4.6 mm ×5μm） column and a mixture of CH3CN-0.02 mol/L CH3COONa as mobile phase for gradient elution. The incidence light wavelength was 233 nm, emission wavelength was 600 nm. The fluorescence reaction time was 30 rain. The contents were calculated with an external standard. Results The linearity was good in the ranges of 10-500 I, Lg/L for EC. The average recovery rates of EC was 93.7% - 106.0%. The RSD was 1.4% - 2.8% , and the limit of quantification was 15 μg/L. GC-MS and HPLC-FLD were compared to evaluate for determining EC content in wine. Conclusion The HPLC-FLD method was simple, accurate and suitable for the determination of EC in multitudinous wine.
出处
《卫生研究》
CAS
CSCD
北大核心
2014年第1期121-124,共4页
Journal of Hygiene Research
基金
国家重点基础研究发展计划(973计划)项目(No.2012CB720804)
