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改进QuEChERS-气相色谱-质谱法测定苹果中胺鲜酯残留
引用本文:孔祥吉,孔顺,张雪梅,孔德洋.改进QuEChERS-气相色谱-质谱法测定苹果中胺鲜酯残留[J].色谱,2019,37(12):1363-1367.
作者姓名:孔祥吉  孔顺  张雪梅  孔德洋
作者单位: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
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  
收稿时间:2019-08-17

Determination of diethyl aminoethyl hexanoate residues in apples by gas chromatography-mass spectrometry combined with improved QuEChERS
KONG Xiangji,KONG Shun,ZHANG Xuemei,KONG Deyang.Determination of diethyl aminoethyl hexanoate residues in apples by gas chromatography-mass spectrometry combined with improved QuEChERS[J].Chinese Journal of Chromatography,2019,37(12):1363-1367.
Authors:KONG Xiangji  KONG Shun  ZHANG Xuemei  KONG Deyang
Institution: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
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.
Keywords:gas chromatography-mass spectrometry (GC-MS)  QuEChERS  diethyl aminoethyl hexanoate (DA-6)  apple  
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