QuEChERS-气相色谱-质谱法测定粮谷中氰烯菌酯残留 |
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引用本文: | 杨金川,张建,白雪梅.QuEChERS-气相色谱-质谱法测定粮谷中氰烯菌酯残留[J].农药学学报,2020,22(6):1099-1103. |
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作者姓名: | 杨金川 张建 白雪梅 |
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作者单位: | 贵州省产品质量检验检测院,贵阳 550001;贵州省市场监督管理局,贵阳 550001 |
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摘 要: | 建立了一种适用QuEChERS前处理结合气相色谱-质谱 (GC-MS) 技术测定4种粮谷(糙米、小麦、高粱及玉米)中氰烯菌酯残留的方法。样品经乙腈提取、PSA净化和浓缩后,采用GC-MS检测,内标法定量。结果表明:在10~500 μg/L质量浓度范围内,氰烯菌酯峰面积与进样质量浓度间线性关系良好,决定系数 (R2) > 0.9983,定量限 (LOQ) 低于0.005 mg/kg;在添加水平分别为0.005、0.02、0.05及0.1 mg/kg时,该方法的平均回收率在85%~108%之间,相对标准偏差 (RSDs) 为1.1%~10.4%。该方法简便、快速,具有良好的灵敏度和重现性,适用于粮谷中氰烯菌酯的残留量测定。
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关 键 词: | 氰烯菌酯 QuEChERS 气相色谱-质谱 残留 检测 粮谷 |
收稿时间: | 2020-01-09 |
Determination of phenamacril in cereals by QuEChERS-gas chromatography-mass spectrometry |
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Institution: | 1.Institution of Supervision and Inspection Product Quality of Guizhou Province, Guiyang 550001, China2.Administration for Market Regulation of Guizhou Province, Guiyang 550001, China |
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Abstract: | A method was developed for the determination of phenamacril residue in four kinds of cereals (rice, wheat, sorghum, corn) by QuEChERS combined with gas chromatography-mass spectrometry (GC-MS). The samples were extracted with acetonitrile, cleaned-up with PSA, concentrated, and detected by GC-MS using internal standard method. The results showed that the linear relationship of phenamacril in the linear range from 10 to 500 μg/L was good, the linear correlation coefficients (R2) was higher than 0.998 3, with the limit of quantitation (LOQs) lower than 0.005 mg/kg. The average recoveries at four spiking levels (0.005 mg/kg, 0.02 mg/kg, 0.05 mg/kg, 0.1 mg/kg) in cereals ranged from 85% to 108%, and the relative standard deviations (RSDs) were from 1.1% to 10.4%. This method was simple, rapid, sensitive and applicable to the determination of phenamacril in cereals. |
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