食品科学

• 安全检测 • 上一篇    下一篇

气相色谱-串联质谱法快速测定水果中咪鲜胺及其代谢物2,4,6-三氯苯酚的残留量

卢俊文,李 蓉*,杨 芳,黄思允,陈丽斯   

  1. 中山出入境检验检疫局,广东 中山 528403
  • 出版日期:2015-06-25 发布日期:2015-06-12
  • 通讯作者: 李 蓉
  • 基金资助:

    广东检验检疫局科技计划项目(2013GDK27);国家质检总局科技计划项目(2015IK260)

Rapid Determination of Residues of Prochloraz and Its Metabolite 2,4,6-Trichlorophenol in Fruits Using Gas Chromatography with Tandem Mass Spectrometry

LU Junwen, LI Rong*, YANG Fang, HUANG Siyun, CHEN Lisi   

  1. Zhongshan Entry-Exit Inspection and Quarantine Bureau, Zhongshan 528403, China
  • Online:2015-06-25 Published:2015-06-12
  • Contact: LI Rong

摘要:

目的:建立基质分散固相萃取-气相色谱-串联质谱法快速测定水果中咪鲜胺及其代谢物2,4,6-三氯苯酚残留量的方法。方法:采用以乙腈作提取剂、以N-丙基乙二胺和十八烷基硅烷键合硅胶(C18)作为混合固相基质分散萃取净化剂的前处理方法,并利用气相色谱-串联质谱在多反应离子监测模式条件下进行检测,用基质匹配标准品的外标法定量。结果:咪鲜胺及其代谢物2,4,6-三氯苯酚在0.004~0.400 mg/kg范围内线性关系均良好,相关系数分别为0.999 4和0.999 2;在3 个添加水平(0.01、0.02、0.10 mg/kg)范围内的平均回收率分别为80.1%~101.5%和79.0%~97.4%,相对标准偏差分别为2.8%~6.8%和2.0%~6.0%,方法的定量限分别为0.004 mg/kg和0.005 mg/kg。结论:该方法前处理简单快速、灵敏度高、测定线性范围宽,可用于水果中咪鲜胺及其代谢物2,4,6-三氯苯酚残留的快速测定。

关键词: 气相色谱-串联质谱, 基质分散固相萃取, 咪鲜胺, 2, 4, 6-三氯苯酚, 水果, 残留

Abstract:

Purpose: To develop a rapid method for the determination of residues of prochloraz and its metabolite,
2,4,6-trichlorophenol, in fruits using matrix dispersive solid-phase extraction and gas chromatography with tandem mass
spectrometry (GC-MS-MS). Methods: Samples were extracted with acetonitrile, cleaned by matrix dispersive solid-phase
extraction using PSA and C18, detected by GC-MS-MS under multiple reaction monitoring mode, and quantified by an
external standard method using matrix-match standard solution. Results: In the linear range of 0.004-0.400 mg/kg, the
correlation coefficients for prochloraz and 2,4,6-trichlorophenol were 0.999 4 and 0.999 2, respectively. Their average
recoveries at spiked levels of 0.01, 0.02 and 0.10 mg/kg were 80.1%–101.5% and 79.0%-97.4% with relative standard
deviations of 2.8%–6.8% and 2.0%–6.0%, respectively, and their limits of quantification (LOQ) (RSN = 10) were 0.004 and
0.005 mg/kg, respectively. Conclusions: The proposed method is simple and sensitive with a wide range of measurement,
and can be suitable for the analysis of prochloraz and 2,4,6-trichlorophenol residues in fruits.

Key words: gas chromatography with tandem mass spectrometry (GC-MS-MS), matrix dispersive solid-phase extraction, prochloraz, 2,4,6-trichlorophenol, fruit, residue

中图分类号: