全自动凯式定氮仪-超高效液相色谱法测定啤酒中甲醛的残留量  

Determination of formaldehyde residues in beer by kjeltec auto analyzer-UPLC

作　　者：张博 石矛 马杰 李青 刘思洁 

机构地区：[1]吉林省卫生检测检验中心,吉林长春130062

出　　处：《中国卫生检验杂志》2015年第3期326-329,共4页Chinese Journal of Health Laboratory Technology

摘　　要：目的建立全自动凯式定氮仪-超高效液相色谱法测定啤酒中甲醛残留量的检测技术。方法采用全自动凯式定氮仪代替传统水蒸汽蒸馏法提取啤酒中的甲醛,经2,4-二硝基苯肼衍生后,生成苯腙类化合物。超高效液相色谱分离,外标法定量。色谱条件为:流动相:乙腈-水(60∶40,V/V)溶液;紫外检测器波长:355 nm。结果通过实验证明,浓度为0μg/ml^10μg/ml时,标准曲线线性关系良好,线性相关系数r为0.999 5。精密度、准确度符合检测要求。相对标准偏差(RSD)为0.6%~2.5%,加标回收率为87.6%~95.7%。结论本方法采取全自动凯式定氮法代替传统蒸馏法,并利用超高效液相色谱仪作为最终检测方法,可检测啤酒中微量的甲醛,具有灵敏度高、选择性好、精密度和准确度好等优点,而且更简便、更快捷,适合对大批量啤酒进行分析检测。Objective To establish a kjeltec auto analyzer- ultra performance liquid chromatography（ UPLC） method for determination of formaldehyde residues in beer. Methods Kjeltec auto analyzer was used to extract formaldehyde in beer instead of traditional steam distillation. Formaldehyde can produce phenylhydrazone by reacting with 2,4- dinitrophenylhydrazine. Mixtrue was separated by UPLC and quantified with external standard. Chromatography conditions were acetonitrile- water（ 60∶40,V/V）,the UV detection wavelength was 355 nm. Results The experiment improved that linear range of determination for formaldehyde was good when the concentration was in 0 μg / ml- 10 μg / ml（ r = 0. 9995）. Both precision and accuracy met the requirements of experiments. The relative standard derivation for formaldehyde was 0. 6%- 2. 5%,and the recovery of it was 87. 6%- 95. 7%. Conclusion This method innovatively takes the kjeltec auto analyzer instead of traditional steam distillation,and uses UPLC as the final detection method. The method has the advantages of simplicity,rapidity,high sensitivity,good selectivity,excellent precision and accuracy,which can be suitable for mass detection analysis of formaldehyde in beer.

关 键 词：超高效液相色谱 啤酒 全自动凯式定氮仪 甲醛 

分 类 号：O657.72[理学—分析化学]