衍生气相色谱法测定啤酒中甲醛含量方法的优化  

Optimization of Formaldehyde Content Determination in Beer by Derivatization Gas Chromatography

作　　者：李中贤[1] 宋跃 赵灿方 刘小培[1] 王俊伟[1] 余学军[1] LI Zhongxian;SONG Yue;ZHAO Canfang;LIU Xiaopei;WANG Junwei;YU Xuejun(High&New Technology Research Center,Henan Academy of Sciences,Hongzhuan Road,Zhengzhou 450002,China;Zhengzhou Railway Center for Disease Control and Prevention,Zhengzhou 450015,China)

机构地区：[1]河南省科学院高新技术研究中心,郑州450002 [2]郑州铁路疾病预防控制所,郑州450015

出　　处：《河南科学》2021年第2期210-214,共5页Henan Science

基　　金：国家自然科学基金-河南省人才培养联合基金(U1404206)。

摘　　要：以2,4-二硝基苯肼作衍生剂,在盐酸溶液中对啤酒样品中的甲醛进行衍生、超声提取,应用正交试验设计通过改变衍生剂用量、衍生温度和衍生时间3个研究因素,对啤酒的前处理条件进行了优化,寻求最佳前处理条件.以峰面积作为衍生化效果评价指标,利用气相色谱-电子捕获检测器(ECD)分离检测,建立了气相色谱法测定啤酒中的甲醛.结果表明,衍生剂用量2.0 mL、衍生温度65℃和衍生时间30 min条件下效果最佳,甲醛在0~2 mg/L的质量浓度范围内具有良好的线性关系,相关系数均大于0.9995.甲醛平均加标回收率在87.3%~99.7%之间,相对标准偏差(RSD)为1.34%~2.24%.该方法操作简单快速、分离度好、准确度高,满足相关检测规范要求,适用于啤酒中甲醛含量的检测.Using 2,4-dinitrophenylhydrazine as derivatization agent,formaldehyde in beer samples was derivatized and ultrasonic extracted in hydrochloric acid solution.Orthogonal test design was used to optimize the pretreatment conditions of beer by changing the amount of derivatization agent,derivatization temperature and derivatization time.The peak area was used as the evaluation index of derivatization effect to seek the best pretreatment conditions.A method for the determination of formaldehyde in beer by gas chromatography with electron capture detector(ECD)was developed.The results showed that the best derivatization conditions were as follows:the amount of derivatization agent 2.0 mL,the temperature 65℃and the time 30 min.The concentrations of formaldehyde presented a good linear relationship with peak area when they were within 0-2 mg/L,and the correlation coefficient of the calibration curve was 0.9995.The recovery rates of formaldehyde were in the range of 87.3%-99.7%and the relevant standard deviations(RSDs)were in the range of 1.34%-2.24%.The method is simple,fast,accurate,and is suitable for the detection of low concentration of formaldehyde in beer.

关 键 词：气相色谱法 甲醛 啤酒 衍生 正交试验 

分 类 号：O657.71[理学—分析化学]