色谱

色谱 ›› 2019, Vol. 37 ›› Issue (12): 1363-1367.DOI: 10.3724/SP.J.1123.2019.08021

• 研究论文 • 上一篇    下一篇

改进QuEChERS-气相色谱-质谱法测定苹果中胺鲜酯残留

孔祥吉1, 孔顺2, 张雪梅3, 孔德洋1   

  1. 1.生态环境部部南京环境科学研究所, 江苏 南京 210042;
    2.东南大学土木工程工程学院, 江苏 南京 211189;
    3.江苏省计量科学研究院, 江苏 南京 210023
  • 收稿日期:2019-08-17 出版日期:2019-12-08 发布日期:2020-12-11
  • 通讯作者: 张雪梅.Tel:(025)86435532,E-mail:11921435@qq.com.

Determination of diethyl aminoethyl hexanoate residues in apples by gas chromatography-mass spectrometry combined with improved QuEChERS

KONG Xiangji1, KONG Shun2, ZHANG Xuemei3, KONG Deyang1   

  1. 1. Nanjing Institute of Environmental Science, Ministry of Ecology and Environment of the People's Republic of China, Nanjing 210042, China;
    2. School of Civil Engineering, Southeast University, Nanjing 211189, China;
    3. Jiangsu Institute of Metrology, Nanjing 210023, China
  • Received:2019-08-17 Online:2019-12-08 Published:2020-12-11

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摘要： 以改进的QuEChERS前处理技术结合气相色谱-质谱（GC-MS）技术，建立了苹果中胺鲜酯残留的检测方法，为苹果中胺鲜酯残留限量的制定提供依据。采用温水作为提取溶剂，提取液经二氯甲烷反萃取，旋转蒸发浓缩、定容净化后，以HP-5MS毛细管柱进行分离，在电子轰击（EI）源、选择离子监测（SIM）模式下检测苹果中胺鲜酯。在3个添加水平下，胺鲜酯的回收率为74.1%~84.2%，相对标准偏差（RSD）为1.5%~4.1%，检出限和定量限分别为0.0024 mg/L和0.008 mg/kg。该方法用于苹果中胺鲜酯残留的检测，灵敏度高，实用性强。

关键词: 气相色谱-质谱, QuEChERS, 胺鲜酯, 苹果

Abstract: A method was developed for the determination of diethyl aminoethyl hexanoate (DA-6) residues in apples by gas chromatography-mass spectrometry (GC-MS) combined with improved QuEChERS. The samples were first extracted with warm water, then, the extract was subjected to liquid-liquid re-extraction with dichloromethane, followed by rotary evaporation concentration. The residues were cleaned up with primary secondary amine (PSA). The analytes were separated on an HP-5 capillary column and detected using an EI source in the SIM mode. The recoveries ranged from 74.1% to 84.2% at three spiked levels, with relative standard deviations (RSDs) between 1.5% and 4.1%. The limit of detection and limit of quantification were 0.0024 mg/kg and 0.008 mg/kg, respectively. The developed method is sensitive, and practically applicable for the determination of DA-6 residues in apple samples.

Key words: gas chromatography-mass spectrometry (GC-MS), QuEChERS, diethyl aminoethyl hexanoate (DA-6), apple

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