论文部分内容阅读
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Agilent TC-C18色谱柱(250 mm×4.6 mm×5μm)分离,乙腈-0.02mol/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233 nm,发射波长为600 nm,衍生化反应时间30 min,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10~500μg/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 establish a high performance liquid chromatography-fluorescence detector (HPLC-FLD) method for the determination of urethane (EC) content in wine. Methods The wine samples were derivatized with 9-hydroxytoluene and analyzed by high performance liquid chromatography-fluorescence with Agilent TC-C18 column (250 mm × 4.6 mm × 5 μm). The acetonitrile-0.02 mol / L sodium acetate solution was flowed Phase and gradient elution. The excitation wavelength of the fluorescence detector was 233 nm, the emission wavelength was 600 nm, the derivatization reaction time was 30 min, and the content was calculated by external standard method. The reliability of HPLC-FLD method was evaluated by GC-MS method . Results EC in the range of 10 ~ 500μg / L showed a good linear relationship with the average recovery of 93.7% ~ 106.0%, the relative standard deviation of 1.4% -2.8%, and the limit of quantification of 15μg / L. HPLC-FLD and GC-MS two methods for the determination of the EC content of wine no significant difference. Conclusion HPLC-FLD is suitable for the rapid determination of EC in wine.