食品科学 ›› 2011, Vol. 32 ›› Issue (22): 280-284.doi: 10.7506/spkx1002-6630-201122060

• 分析检测 • 上一篇    下一篇

HPLC-MS/MS测定玉米中异恶唑草酮及代谢物残留量

杨长志,王传松,程 阳,刘 永,吴 岩,魏冬旭   

  1. 黑龙江出入境检验检疫局
  • 出版日期:2011-11-25 发布日期:2011-11-11
  • 基金资助:
    国家认证认可管理委员会检验检疫行业标准制订项目(2009B412)

Determination of Isoxaflutole and Its Metabolite Residues in Maize by HPLC-MS/MS

YANG Chang-zhi,WANG Chuan-song,CHENG Yang,LIU Yong,WU Yan,WEI Dong-xu   

  1. (Heilongjiang Entry and Exit Inspection and Quarantine Bureau, Harbin 150001, China)
  • Online:2011-11-25 Published:2011-11-11

摘要: 建立玉米中异恶唑草酮及代谢物残留量同时测定的高效液相色谱-串联质谱(high performance liquid chromatorgerphy-mass spectrometry/mass spectrometry,HPLC-MS/MS)分析法。试样用乙酸-乙腈(1:99, V/V)高速匀浆提取、醋酸钠和无水硫酸镁盐析后,提取液经N-丙基乙二胺(PSA)、十八烷基硅烷(ODS)和石墨化炭黑(GCB)净化,除去样品中脂肪和色素等大多数的干扰基质,用高效液相色谱-串联质谱仪检测,外标法定量。异恶唑草酮及代谢物的添加量在0.005~0.100mg/kg范围内,样品平均加标回收率在74.8%~107.2%之间,相对标准偏差为6.45%~11.15%;方法的检测限异恶唑草酮为0.01mg/kg、异恶唑草酮代谢物0.005mg/kg。本方法灵敏、准确、省时和操作简便,适用于玉米中异恶唑草酮及代谢物残留量同时检测和确证。

关键词: 异恶唑草酮及代谢物, 液相色谱-串联质谱, 玉米

Abstract: An HPLC-MS/MS (high performance liquid chromatography coupled with tandem mass spectrometry) method has been developed for the determination of isoxaflutole and its two metabolite residues in maize. The isoxaflutole and its metabolite residues in samples were extracted into acetic acid-cetonitrile (1:99, V/V) by means of high-speed homogenization, subjected to liquid-liquid partition in the presence of added anhydrous magnesium sulfate and sodium acetate, cleaned up with primary secondary amine (PSA), octadecylsilane (ODS) and graphitized carbon black for purpose of eliminating such most matrix interferences as lipids, pigments, etc before HPLC-MS/MS analysis and subsequent quantification by an external standard method. The average recovery rates of isoxaflutole and its metabolites from spiked samples ranged between 74.8% and 107.2% with a relative standard deviation of 6.45%-11.15% across the spike levels of 0.010, 0.050 mg/kg and 0.100 mg/kg. The detection limit was 0.01 mg/kg and 0.005 mg/kg for isoxaflutole and its metabolites, respectively. This method was sensitive, accurate, time-saving, simple, and suitable for the detection of isoxaflutole and its metabolite residues in maize.

Key words: isoxaflutole and its metabolites, high performance liquid chromatography coupled with tandem mass spectrometry(HPLC-MS/MS), maize

中图分类号: