衍生化气质联用法测定空气中甲醛  

Derivatized gas chromatography-mass spectrometry method for determination of formaldehyde in air

作　　者：郑三燕[1] 方美璇 马奇发 林彩琴[1] 陈珞洛[1] ZHENG San-yan;FANG Mei-xuan;MA Qi-fa;LIN Cai-qin;CHEN Luo-luo(Wenzhou Municipal Center for Disease Control and Prevention,Wenzhou,Zhejiang 325000,China)

机构地区：[1]温州市疾病预防控制中心,浙江325000

出　　处：《中国卫生检验杂志》2022年第22期2711-2713,2719,共4页Chinese Journal of Health Laboratory Technology

基　　金：温州市基础性公益科研项目(Y20210385)。

摘　　要：目的采用2,4-二硝基苯肼衍生,气相色谱质谱联用检测,建立-种快速、简便、便于推广的空气中甲醛检测方法。方法选用2.0 g/L浓度的2.4-二硝基苯肼作为衍生剂,加入0.2 ml于样品中,与样品中甲醛在60℃下反应30 min生成衍生产物2,4-二硝基苯腙,经DB-5MS毛细管色谱柱分离,采用气相色谱质谱联用方法定性检测甲醛的衍生化合物,外标曲线法定量。结果甲醛在0.01μg/ml~0.5μg/ml内线性关系良好,相关系数为0.9996,添加低、中、高3个不同浓度水平,经测定回收率均在95.65%~100.00%,相对标准偏差为1.0%,最低检出浓度和最低定量浓度分别为0.005 mg/m^(3)和0.015 mg/m^(3)。用上述建立的方法检测了多份室内空气样品,其含量范围为0.008 mg/m^(3)~0.12 mg/m^(3)。结论该检测方法操作简单、方便,回收率与精密度均符合要求,可用于空气中甲醛的检测。Objective A rapid,simple and convenient method for the detection of formaldehyde in air was established by gas chromatography-mass spectrometry(GC-MS)derived from 2,4-dinitrophenylhydrazine.Methods The 2.4-dinitrophenylhydrazine with a concentration of 2.0 g/L was used as a derivative,and 0.2 ml was added to the sample,which reacted with formaldehyde in the sample at 60℃for 30 min.The derivatives were separated by DB-5 MS capillary chromatographic column.The derivatives of formaldehyde were qualitatively detected by GC-MS and quantified by external standard curve method.Results A good linearity was observed at the concentration of 0.01 mg/L-0.50 mg/L,with correlation coefficient(r)greater than 0.9996.The recovery rates at three spiking levels were 95.65%-100.00%,and the relative standard deviation(RSD)was below 1.0%.The lowest detection concentration and the lowest quantitative concentration were 0.005 mg/m^(3) and 0.015 mg/m^(3),respectively.A number of indoor air samples were detected by the above established method,and the content ranged from 0.008 mg/m^(3) to 0.12 mg/m^(3).Conclusion The detection method is simple and convenient,and the recovery and precision meet the requirements.It can provide a reference method for the detection of formaldehyde in air.

关 键 词：甲醛 衍生化 气质联用 空气 

分 类 号：O657[理学—分析化学]