引用本文:
苏建峰, 钟茂生, 张光军, 陈竞秀, 林立峰, 刘建军. 固相萃取-气相色谱-质谱联用测定葱属蔬菜中二甲嘧菌胺和吡氟禾草灵残留量[J]. 应用化学,
2010, 27(5): 590-593.
doi:
10.3724/SP.J.1095.2010.90529
Citation: SU Jian-Feng, ZHONG Mao-Sheng, ZHANG Guang-Jun, CHEN Jin-Xiu, LIN Li-Feng, LIU Jian-Juna. Determination of Residual Pyrimethanil and Fluazifop-butyl in Onion by Gas Chromatography-mass Spectrometry[J]. Chinese Journal of Applied Chemistry, 2010, 27(5): 590-593. doi: 10.3724/SP.J.1095.2010.90529
Citation: SU Jian-Feng, ZHONG Mao-Sheng, ZHANG Guang-Jun, CHEN Jin-Xiu, LIN Li-Feng, LIU Jian-Juna. Determination of Residual Pyrimethanil and Fluazifop-butyl in Onion by Gas Chromatography-mass Spectrometry[J]. Chinese Journal of Applied Chemistry, 2010, 27(5): 590-593. doi: 10.3724/SP.J.1095.2010.90529
固相萃取-气相色谱-质谱联用测定葱属蔬菜中二甲嘧菌胺和吡氟禾草灵残留量
摘要:
在固相萃取基础上通过极性区间排列净化前处理,建立了固相萃取-气相色谱-质谱法检测青葱、大葱、洋葱中的二甲嘧菌胺与吡氟禾草灵残留的分析方法。样品用乙腈提取,加入氯化钠继续均质,离心分层后取部分乙腈层过Envi-18柱和Florisil柱净化后上机测试。采用选择离子扫描方式,外标法定量。分析方法简便、快速。通过优化前处理和上机条件,在最优条件下进行测试,二甲嘧菌胺与吡氟禾草灵的定量下限(S/N=10)均小于0.01mg/kg,在加标水平0.01~0.2mg/kg范围内,回收率分别为81.4%~94.6%、107%~129%,相对标准偏差分别为3.3%~11%、4.0%~9.7%。
English
Determination of Residual Pyrimethanil and Fluazifop-butyl in Onion by Gas Chromatography-mass Spectrometry
Abstract:
A pretreatment method was developed based on solid phase extraction(SPE) and applied to determine the residual pyrimethanil and fluazifop-butyl in green onion,scallion and onion by gas chromatography-mass spectrometry(GC-MS).The samples were extracted from homogenized tissue with acetonitrile,separated with liquid-liquid partition.The supernatants were purified by SPE(Envi-18 and Florisil columns) prior to the GC-MS analysis.Determination was performed in a selected ion monitoring(SIM) mode and external standard method was used in the quantification.The method was convenient and rapid after investigating the conditions of pretreatment and determination.Under the optimal conditions,the detection limits of pesticides by the method(S/N=10) were under 0.01 mg/kg.Tests for recovery were carried out by addition of standard at a concentration of 0.01~0.2 mg/kg,the recoveries of pyrimethanil and fluazifop-butyl were 81.4%~94.6% and 107%~129% with relative standard deviations of 3.3%~11% and 4.0%~9.7%,respectively.
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