改进QuEChERS-气相色谱-质谱法测定苹果中胺鲜酯残留  

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

作　　者：孔祥吉 孔顺 张雪梅[3] 孔德洋 KONG Xiangji;KONG Shun;ZHANG Xuemei;KONG Deyang(Nanjing Institute of Environmental Science,Ministry of Ecology and Environment of the People’s Republic of China,Nanjing 210042,China;School of Civil Engineering,Southeast University,Nanjing 211189,China;Jiangsu Institute of Metrology,Nanjing 210023,China)

机构地区：[1]生态环境部南京环境科学研究所,江苏南京210042 [2]东南大学土木工程学院,江苏南京211189 [3]江苏省计量科学研究院,江苏南京210023

出　　处：《色谱》2019年第12期1363-1367,共5页Chinese Journal of Chromatography

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0.002 4 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。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 0.002 4 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.

关 键 词：气相色谱-质谱 QUECHERS 胺鲜酯 苹果 

分 类 号：O658[理学—分析化学]