色谱

色谱 ›› 2014, Vol. 32 ›› Issue (1): 69-73.DOI: 10.3724/SP.J.1123.2013.06035

• 研究论文 • 上一篇    下一篇

气相色谱-质谱法同时测定水果中9种保鲜剂的残留量

彭淑女1, 王秋泉1, 方兰兰2, 郭善勇2, 曾舟华2, 林竹光1   

  1. 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
  • 收稿日期:2013-06-19 修回日期:2013-07-25 出版日期:2014-01-08 发布日期:2013-12-26
  • 通讯作者: 林竹光
  • 基金资助:

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

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

PENG Shunü1, WANG Qiuquan1, FANG Lanlan2, GUO Shanyong2, ZENG Zhouhua2, LIN Zhuguang1   

  1. 1. Department of Chemistry & Institute of Analytical Science, College of Chemistry and Chemical Engineering, Xiamen University, Xiamen 361005, China;
    2. Xiamen Tungsten Co., Ltd., Xiamen 361005, China
  • Received:2013-06-19 Revised:2013-07-25 Online:2014-01-08 Published:2013-12-26

PDF

355

被引次数

7

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(1/3，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0.10~2.16 μg/kg，在50、100、200 μg/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。

关键词: 保鲜剂, 农药残留, 气相色谱-质谱, 水果

Abstract:

A gas chromatography-mass spectrometry (GC-MS) method was established for the simultaneous determination of nine typical preservatives (pyrimethanil, chlorothalonil, chlorpyrifos, 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 2.16 μg/kg. The average recoveries were in the range of 75.3% to 128% at the spiked levels of 50, 100 and 200 μg/kg with the relative 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.

Key words: fruits, gas chromatography-mass spectrometry (GC-MS), pesticide residue, preservatives

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