食品科学 ›› 2009, Vol. 30 ›› Issue (12): 202-204.doi: 10.7506/spkx1002-6630-200912044

• 分析检测 • 上一篇    下一篇

超高效液相色谱-串联质谱法测定干香菇中的多菌灵和噻菌灵残留量

连文浩,苏建峰,江滨炜   

  1. 福建华日食品安全检测有限公司
  • 收稿日期:2008-09-04 修回日期:2008-11-22 出版日期:2009-06-15 发布日期:2010-12-29
  • 通讯作者: 连文浩 E-mail:lianwenhao@fairreach.com

Ultra-performance Liquid Chromatography-Tandem Mass Spectrometry for the Determination of Carbendazim and Thiabendazole Residues in Dried Shiitake (Lentinula edodes)

LIAN Wen-hao,SU Jian-feng,JIANG Bin-wei   

  1. (Fujian Fairreach Food Safety Testing Co. Ltd., Fuzhou 350015, China)
  • Received:2008-09-04 Revised:2008-11-22 Online:2009-06-15 Published:2010-12-29
  • Contact: LIAN Wen-hao E-mail:lianwenhao@fairreach.com

摘要:

称取1.0g 干香菇样品,用0.02mol/L 盐酸- 甲醇(80:20,V/V)溶液浸泡提取,调节溶液pH 值至6~8,用二氯甲烷进行提取净化,旋转蒸发器减压蒸干后,用30% 甲醇水溶解,样液用超高效液相色谱分离,电喷雾串联四级杆质谱进行检测,外标法定量。本法研究的多菌灵和噻菌灵的线性范围为1.0~100.0μg/L,线性相关系数R2 > 0.99,在1.0~10.0μg/kg 的3 个添加水平范围内的平均回收率为78%~106%,相对标准偏差为7.9%~9.8%,方法检测限可达1.0μg/kg,在3min 内快速完成分析测试,可应用于大通量的实际样品检测。

关键词: 干香菇, 超高效液相色谱-串联质谱法, 多菌灵, 噻菌灵

Abstract:

A method for simultaneous analysis of carbendazim and thiabendazole in dried shiitake was developed using ultraperformance liquid chromatography coupled with tandem mass spectrometry (UPLC-MS/MS). Sample was extracted with 0.02 mol/L hydrochloric acid solution containing 20% methanol, adjusted pH to 6-8, purified with dichloromethane, dried by rotary evaporator, and dissolved in 30% methanol solution. The sample was detected by the UPLC-MS/MS, and quantified by external standard method. Results showed that the linear ranges for determination of carbendazim and thiabendazole by this method were both between 1.0 μg/L and 100.0 μg/L (R2 > 0.99); the average recoveries for the two pesticides in dried shiitake spiked at three levels (1.0, 5.0 and 10.0 μg/kg) were 78%-106%, and the RSDs were 7.9%-9.8% (n = 6); the limit of detection was 1.0 μg/kg; the method could be quickly finished in 3 min and be applied in large amount detection of samples.

Key words: dried mushroom, ultra-performance liquid chromatography - tandem mass spectrometry (UPLC - MS/MS), carbendazim, thiabendazole

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