色谱

色谱 ›› 2012, Vol. 30 ›› Issue (03): 262-266.DOI: 10.3724/SP.J.1123.2011.10035

• 研究论文 • 上一篇    下一篇

固相萃取-气相色谱串固相萃取-气相色谱-串联质谱法测定水果中11种三唑类杀菌剂

郭萌萌, 谭志军, 吴海燕, 李兆新*, 翟毓秀   

  1. 宁波市疾病预防控制中心 宁波市毒物研究与控制重点实验室, 浙江 宁波 315010
  • 收稿日期:2011-10-28 修回日期:2011-12-06 出版日期:2012-03-28 发布日期:2012-05-02
  • 通讯作者: 李继革,硕士,副主任技师,主要从事理化检验工作. Tel: (0574)87274559
  • 基金资助:

    浙江省医药卫生科学研究基金项目(2011RCB032)

Determination of 11 triazole fungicides in fruits using solid phase extraction and gas chromatography-tandem mass spectrometry

GUO Mengmeng, TAN Zhijun, WU Haiyan, LI Jige*, WANG Yufei, SHI Jiawei, LI Jige*, WANG Yufei, SHI Jiawei, JIANG Li, YAO Xunping, FANG Lanyun   

  1. Ningbo Key Laboratory of Poison Research and Control, Ningbo Municipal Center for Disease Control and Prevention, Ningbo 315010, China
  • Received:2011-10-28 Revised:2011-12-06 Online:2012-03-28 Published:2012-05-02

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摘要： 建立了固相萃取-气相色谱-串联质谱同时测定水果中11种三唑类杀菌剂残留的方法。采用乙腈匀浆提取样品中的待测组分,经固相萃取法(SPE)净化,采用气相色谱-串联质谱在多反应监测(MRM)模式下进行测定,外标法定量。分别对水果样品进行4个水平(10、50、100、250 μg/kg)的加标回收试验,回收率为82.6%～117.1%,相对标准偏差小于10%,定量限(LOQ,以信噪比(S/N)为10计)为0.8～3.4 μg/kg。结果显示该方法的背景干扰低,灵敏度高,定量限低于国家标准及有关文献报道值,适合橘子等水果中三唑类杀菌剂的同时测定。

关键词: 固相萃取, 气相色谱-串联质谱, 三唑类杀菌剂, 水果

Abstract: A method was developed and validated for the simultaneous determination of 11 triazole fungicides （tetraconazole, triflumizole, penconazole, hexaconazole, flutriafol, myclobutanil, etuconazole, propiconazole, tebuconazole, epoxiconazole and fluquinconazole） in fruits by gas chromatography-tandem mass spectrometry (GC-MS/MS). The triazole fungicides were extracted from the samples with acetonitrile, then enriched and cleaned-up with solid phase extraction (SPE) on a Carbon/NH2 cartridge (collecting 2~10 mL effluent). The detection was carried out by GC-MS/MS in the multiple reaction monitoring (MRM) mode, and the quantification analysis was performed by external standard method. The calibration curves showed good linearity in the range of 10~500 μg/L. The correlation coefficients were larger than 0.9940. The average recoveries of the 11 fungicides spiked in the fruits at the levels of 10, 50, 100 and 250 μg/kg were between 82.6% and 117.1%, and the relative standard deviations (RSD) were less than 10%. The limits of quantification (S/N=10) were between 0.8 μg/kg and 3.4 μg/kg. The method possesses low background, high sensitivity, and quantification limits lower than that of the national standard and the values reported in the relevant literature. It can be applied to the routine analysis of the 11 triazole fungicides in fruits.

Key words: fruits, triazole fungicide, gas chromatography-tandem mass spectrometry (GC-MS/MS), solid phase extraction (SPE)