李红洲¹，彭小东¹，陈大鹏¹，谈晓君¹，李本良¹，刘晶晶¹，杨路宽^2*

（1.贵州省产品质量检验检测院，贵州贵阳 550001；

2.贵州科标测试技术有限公司，贵州贵阳 550001）

摘要：建立了一种超高效液相色谱-离子肼质谱联用技术测定米粉中甲醛的方法。采用2，4-二硝基苯肼溶液作为衍生液，将甲醛衍生成甲醛-2，4-二硝基苯腙后，经C18柱分离，采用电喷雾离子源（ESI），多反应监测（MRM）→相关信息扫描（IDA）→增强子离子扫描（EPI）的联合扫描模式，建立甲醛标准对照品数据库，并通过谱库检索，将阳性可疑样品EPI谱图与标准谱库进行对比确证，可有效排除假阳性。在质量浓度为0.01-1 μg/mL的范围内，方法的线性关系良好，相关系数r＞0.995，检出限为0.05 mg/kg，平均回收率为91.7%，RSD为2.08%。该方法前处理简单、灵敏度高、专属性强，能准确地对样品中非法添加的甲醛进行定性和定量测定。

关键词：超高效液相色谱-离子肼质谱联用法；多反应监测（MRM）→相关信息扫描（IDA）→增强子离子扫描（EPI）扫描；米粉；甲醛

中图分类号：TS207.3   文献标识码：A   文章编号：1674-506X（2020）03-0108-0005

Determination of Formaldehyde in Rice Noodles by High Performance Liquid Chromatography Ion-trap Mass Spectrometry

LI Hong-zhou¹, PENG Xiao-dong¹, CHEN Da-peng¹, TAN Xiao-jun¹, LI Ben-liang¹, LIU Jing-jing¹, YANG Lu-kuan^2*

（1.Institution of Inspection and Testing Product Quality of Guizhou Province, Guiyang Guizhou 550001, China;

2.Kebiao Testing Technology Co., Ltd., Guizhou Province, Guiyang Guizhou 550001, China）

Abstract：A method for determination of formaldehyde in rice noodles by super high performance liquid chromatography ion-trap mass spectrometry was established. Formaldehyde in rice noodles was extracted by using 2, 4-dinitrophenylhydrazine solution as derivative, make formaldehyde derivative into formaldehyde-2, 4-dinitrophe-nylhydrazone, the later was separated by C18 column, and analyzed by the electrospray ionization, multiple reaction monitoring and relevant information scanning combined with enhanced ion scanning. The database of formaldehyde-2, 4-dinitrophenylhydrazone standard reference materials was established, and the EPI spectra of the positive suspicious samples were compared with the standard spectra to confirm the results. The relation displayed good linearity at the mass concentration ranged from 0.01 μg/mL to 1 μg/mL, and all correlation coefficients higher than 0.995. The detection limit was 0.05 mg/kg, average recoveries were 91.7%, with relative standard deviation of 2.08%. The method is simple, sensitive and specific, which can be used for the qualitative and quantitative determinations of formaldehyde in rice noodles.

Keywords：high performance liquid chromatography ion-trap mass spectrometry; MRM→IDA→EPI; rice noodles; formaldehyde

doi：10.3969/j.issn.1674-506X.2020.03-021

收稿日期：2020-03-06

作者简介：李红洲（1987-），男，本科，助理工程师。研究方向：食品与化学。

*通讯作者

引文格式：李红洲,彭小东,陈大鹏,等.超高效液相色谱-离子肼质谱联用法测定米粉中甲醛[J].食品与发酵科技,2020,56(3):108-112.