改良的QuEChERS结合气相色谱-质谱法测定新鲜水果和肉中肉桂醛残留

doi:10.3724/SP.J.1123.2017.11035

色谱 ›› 2018, Vol. 36 ›› Issue (6): 541-546.DOI: 10.3724/SP.J.1123.2017.11035

• 生物基质农兽药残留检测专栏 • 上一篇下一篇

改良的QuEChERS结合气相色谱-质谱法测定新鲜水果和肉中肉桂醛残留

刘萤, 张蓉, 崔凤云, 韩深

北京出入境检验检疫局检验检疫技术中心, 北京 100026

收稿日期:2017-11-21 出版日期:2018-06-08 发布日期:2014-04-24
通讯作者: 韩深,Tel:(010)58619233,E-mail:hansh@bjciq.gov.cn
基金资助:
食品安全国家标准制定项目（spaq-2016-179）.

Determination of cinnamaldehyde residues in fresh fruits and meats by modified QuEChERS combined with gas chromatography-tandem mass spectrometry

LIU Ying, ZHANG Rong, CUI Fengyun, HAN Shen

Inspection and Quarantine Technical Center of Beijing Entry-Exit Inspection and Quarantine Bureau, Beijing 100026, China

Received:2017-11-21 Online:2018-06-08 Published:2014-04-24
Supported by:
National Food Safety Standard Establishment Project (No.spaq-2016-179).

摘要/Abstract

摘要：

建立了改良的QuEChERS技术结合气相色谱-质谱检测水果和肉中肉桂醛残留量的定性定量分析方法。试样用乙酸乙酯溶液均质提取，经N-丙基乙二胺（PSA）、石墨化炭黑（GCB）、C₁₈固相吸附剂净化，在电子轰击电离（EI）源、选择离子监测（SIM）模式下检测，外标法定量。肉桂醛在0.01~0.5 mg/L范围内线性关系良好，相关系数大于0.999。水果和鲜肉中肉桂醛的定量限分别为0.5 mg/kg和1.0 mg/kg。在3个添加水平下，肉桂醛的加标回收率为81.9%~104.5%，相对标准偏差（RSD，n=6）为1.1%~8.6%。该方法操作简单，净化效果好，适用于水果和鲜肉中肉桂醛残留量的快速检测。

关键词: QuEChERS, 气相色谱-质谱, 肉, 肉桂醛, 水果

Abstract:

A method for the determination of cinnamaldehyde residues in fresh fruits and meats by gas chromatography-tandem mass spectrometry (GC-MS) coupled with modified QuEChERS was developed. The samples were extracted with ethyl acetate. Solid phase extraction agents such as graphitized carbon black (GCB), primary-secondary amine (PSA) and octadecyl bonded silica (C₁₈) were used for adsorption and purification. The extracts were detected by electron impact ionization in selected ion monitoring (SIM) mode and quantified using external standard method. The results revealed correlation coefficients (R²) greater than 0.999 in the range of 0.01-0.5 mg/L. The limits of quantification (LOQs) were 0.05 to 0.1 mg/kg. The recoveries at the three spiked levels ranged from 81.9% to 104.5% with the relative standard deviations (RSDs) ranging from 1.1% to 8.6%. The proposed method is efficient, sensitive, reliable, and is suitable for the trace determination of the cinnamaldehyde residues in fresh fruits and meats.

Key words: cinnamaldehyde, fruit, gas chromatography-tandem mass spectrometry (GC-MS), meat, QuEChERS

中图分类号:

O658

刘萤, 张蓉, 崔凤云, 韩深. 改良的QuEChERS结合气相色谱-质谱法测定新鲜水果和肉中肉桂醛残留[J]. 色谱, 2018, 36(6): 541-546.

LIU Ying, ZHANG Rong, CUI Fengyun, HAN Shen. Determination of cinnamaldehyde residues in fresh fruits and meats by modified QuEChERS combined with gas chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2018, 36(6): 541-546.

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改良的QuEChERS结合气相色谱-质谱法测定新鲜水果和肉中肉桂醛残留

Determination of cinnamaldehyde residues in fresh fruits and meats by modified QuEChERS combined with gas chromatography-tandem mass spectrometry

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