气相色谱-质谱法同时测定水果中9种保鲜剂的残留量  

Simultaneous determination of nine preservatives in fruits using gas chromatography-mass spectrometry

作　　者：彭淑女[1] 王秋泉[1] 方兰兰 郭善勇 曾舟华 林竹光[1] 

机构地区：[1]厦门大学化学化工学院化学系,分析科学研究所,福建厦门361005 [2]厦门钨业股份有限公司,福建厦门361005

出　　处：《色谱》2014年第1期69-73,共5页Chinese Journal of Chromatography

基　　金：国家重点基础研究发展计划(“973”)项目(2009CB421605)

摘　　要：建立了采用气相色谱-质谱（GC—MS）同时测定水果中9种保鲜剂残留量的分析方法。水果样品用正己烷／乙酸乙酯（1／1，v／v）混合提取剂超声提取，经Florisil层析柱净化后用正己烷／乙酸乙酯（113，v／v）混合洗脱剂洗脱，以磷酸三苯脂（TPP）为内标物，采用GC—MS的全扫描方式（SCAN）和选择离子监测方式（SIM）对9种保鲜剂进行定性与定量分析。实验结果表明，9种保鲜剂的检出限（LOD）为0．10～2．16μg／kg，在50、100、200μg／kg添加水平下的回收率为75．3％～128％，相对标准偏差为1．57％-11．6％。本分析方法样品前处理简便，净化效果明显，在SIM谱图中分析目标物响应值大、灵敏度高，定量准确可靠，能够满足保鲜剂痕量残留的检测要求。A gas chromatography-mass spectrometry （GC-MS） method was established for the simultaneous determination of nine typical preservatives （pyrimethanil, chlorothalonil, chlor- pyrifos, triadimefon, thiabendazole, imazalil, myclobutanil, iprodione, prochloraz ） in fruits. The fruit samples were subjected to ultrasonic extraction with hexane/ethyl acetate （1/1, v/v）, and followed by purification using diatomite column chromatography with hexane/ethyl acetate （1/3, v/v） eluant. Qualitative and quantitative analysis of the nine preservatives were performed on the GC-MS at full-scan （ SCAN ） and selected ion monitoring （ SIM ） modes, in which triphenylphosphate was used as the internal standard. The detection limits obtained for the nine preservatives were ranged from 0. 10 μg/kg to 2. 16μg/kg. The average recoveries were in the range of 75.3% to 128% at the spiked levels of 50, 100 and 200μg/kg with the rel- ative standard deviations （RSDs） of 1.57% to 11.6% （n = 5 ）. The results showed that the developed method is sensitive and accurate for the determination of the nine preservatives in fruits.

关 键 词：气相色谱-质谱 保鲜剂 水果 农药残留 

分 类 号：O658[理学—分析化学]