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

作　　者：田双双 张琪 庄美慧 詹子悦 赵紫微[1] 谢继安[1] 刘柏林[1] TIAN Shuang-Shuang;ZHANG Qi;ZHUANG Mei-Hui;ZHAN Zi-Yue;ZHAO Zi-Wei;XIE Ji-An;LIU Bo-Lin(Anhui Provincial Center for Disease Control and Prevention,Hefei 230601,China)

机构地区：[1]安徽省疾病预防控制中心,合肥230601

出　　处：《食品安全质量检测学报》2024年第14期133-138,共6页Journal of Food Safety and Quality

基　　金：安徽省卫生健康委科研一般项目(AHWJ2022b089)。

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C_(18)吸附剂净化,经XBridge C_(18)(250 mm×4.6 mm,5μm)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10μL。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0.02~250.00μg/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。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 C_(18)power,separated by XBridge C_(18)(250 mm×4.6 mm,5μm)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 10μL.Results A good linearity of 4 kinds of fragrance enhancers was obtained in the range of 0.02–250.00μg/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.

关 键 词：香兰素 甲基香兰素 乙基香兰素 香豆素 糖果 

分 类 号：O657.72[理学—分析化学] TS246.57[理学—化学]