液相色谱-串联质谱法测定水果中8种极性农药残留量
目的 建立高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry, HPLC-MS/MS)同时测定水果中8种极性农药残留量的分析方法。方法 样品采用含1%(V:V)乙酸的乙腈溶液提取后, 以PC-HILLIC色谱柱分离待测物, 采用鞘流电喷雾离子化, 正离子扫描和多反应监测模式(multiple reaction monitoring, MRM)检测, 基质匹配标准溶液外标法定量。结果 野燕枯、灭蝇胺和助壮素在0.1~200 μg/L之间, 矮壮素在0.1~500 μg/L, 丁酰肼在1~500 μg/L, 沙蚕毒素在2~1000 μg/L, 敌草快和百草枯在5~1000 μg/L范围内线性关系良好, 相关系数均大于0.990。8种极性农药的方法定量限在0.1~20.0 μg/kg 之间, 样品添加回收试验的平均回收率为73.6%~118.5%, 相对标准偏差(relative standard deviation, RSD)(n=6)在3.4%~17.4%之间。结论 该方法快速简便, 定量准确, 可满足多种水果中8种极性农药的残留检测要求。
Objective To establish a method for the simultaneous determination of 8 kinds of polar pesticides residues in fruits by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Methods The samples were extracted with acetonitrile containing 1% (V:V) acetic acid, separated on a PC-HILLIC column, ionized by sheath hydroelectricity spray, and detected by positive ion scanning and multiple reactions monitoring (MRM) mode. The matrix-matched external standard calibration curves were used for quantitative analysis. Results Difenzoquat, cyromazine and mepiquat had good linear relationship in the concentration ranges of 0.1-200 μg/L, chlormequatin, daminozide, nereistoxin had good relationship in the concentration range of 0.1- 500 μg/L, 1.0-500 μg/L and 2.0-1000 μg/L, respectively. Diquat and paraquat had good in the concentration ranges of 5-1000 μg/L. The correlation coefficients were higher than 0.990. The limits of quantification of the method were 0.1-20.0 μg/kg. For all the samples, the average spiked recoveries ranged from 73.6% to 118.5%, and the relative standard deviations (RSDs, n=6) were in the range of 3.4%-17.4%. Conclusion This method is quick, easy, effective, sensitive and accurate, which can meet the requirements for the determination of the 8 kinds of polar pesticides residues in fruits.
标题：液相色谱-串联质谱法测定水果中8种极性农药残留量
英文标题：Determination of 8 kinds of polar pesticides residues in fruits by high performance liquid chromatography-tandem mass spectrometry
作者：
黄何何 厦门出入境检验检疫局检验检疫技术中心
吴媛 厦门出入境检验检疫局检验检疫技术中心
徐敦明 厦门出入境检验检疫局检验检疫技术中心
中文关键词:QuEChERS,高效液相色谱-串联质谱法,极性农药,水果,
英文关键词:QuEChERS,high performance liquid chromatography-tandem mass spectrometry,polar pesticides residues,fruits,
发表日期：2018-08-17
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