分散固相萃取-高效液相色谱法同时测定巧克力糖果中4种增香剂

Simultaneous determination of 4 kinds of flavor enhancer in chocolate candy by dispersion solid phase extraction-high performance liquid chromatography

中文关键词:  香兰素  甲基香兰素  乙基香兰素  香豆素  糖果

英文关键词:vanillin  3,4-dimethoxybenzaldehyde  ethyl vanillin  coumarin  candy

中文摘要:

      目的 建立分散固相萃取-高效液相色谱法同时测定巧克力糖果中香兰素、甲基香兰素、乙基香兰素和香豆素4种增香剂含量的分析方法。方法 实验样品经0.1%甲酸-乙腈提取后, 经C18吸附剂净化, 经XBridge C18 (250 mm×4.6 mm, 5 μm)色谱柱分离, 以甲醇-乙腈(80:20, V:V)溶液(A)和0.1%甲酸-水(V:V)溶液(B)为流动相, 梯度洗脱, 流速1.0 mL/min, 柱温度为30℃, 测定波长297 nm, 进样体积为10 μL。以色谱保留时间定性, 标准曲线法定量。结果 4种增香剂在质量浓度为0.02~250.00 μg/mL范围内与峰面积呈现良好的线性关系(r>0.999), 定量限(limits of quantitation, LOQs)均为0.15 mg/kg。以巧克力糖果为基质, 低中高3浓度水平进行加标回收实验, 4种增香剂的平均回收率为76.6%~99.1%, 相对标准偏差(relative standard deviations, RSDs)为0.9%~4.4% (n=6)。结论 该方法样品前处理简便、快速, 准确度高, 精密度好, 适用于批量巧克力糖果中香兰素、甲基香兰素、乙基香兰素和香豆素含量的快速测定。

英文摘要:

      Objective To establish a method for simultaneous determination of vanillin, 3,4-dimethoxybenzaldehyde, ethyl vanillin and coumarin in chocolate candy by dispersion solid phase extraction-high performance liquid chromatography. Methods The samples were extracted by 0.1% formic acid-acetonitrile, purified by C18 power, separated by XBridge C18 (250 mm×4.6 mm, 5 μm) column. Gradient elution was performed by methanol-acetonitrile (80:20, V:V) solution (A) and 0.1% formic acid-aqueous solution (B) as mobile phase with the flow rate of 1.0 mL/min. The column temperature was 30℃, the determination wavelength was 297 nm, and the sample injection volume was 10 μL. Results A good linearity of 4 kinds of fragrance enhancers was obtained in the range of 0.02–250.00 μg/mL (r>0.999), the limits of quantitation (LOQs) were 0.15 mg/kg. And the chocolate candy as the matrix, the average recoveries of 4 kinds of fragrance enhancers in chocolate confections were 76.6%–98.8% at low, middle and high standard concentration levels, the relative standard deviations (RSDs) were 0.9%-4.4% (n=6). Conclusion This method has the advantages of simple operation, rapid, high accuracy and good precision, suitable for the rapid determination of vanillin, 3,4-dimethoxybenzaldehyde, ethyl vanillin and coumarin in bulk chocolate confectionery.