QuEChERS-高效液相色谱-串联质谱法测定主要谷物和油料作物中氯虫苯甲酰胺的残留
投稿时间:2017-11-03      点此下载全文 HTML
引用本文:马婧玮,马欢,安莉,吴家锴,汪红,祁玉峰,陈寅,吴绪金,等.QuEChERS-高效液相色谱-串联质谱法测定主要谷物和油料作物中氯虫苯甲酰胺的残留[J].农药学学报,2018,20(1):129-134.
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马婧玮 河南省农业科学院 农业质量标准与检测技术研究所/河南省粮食质量安全与检测重点实验室/农业部农产品质量安全风险评估实验室(郑州), 郑州 450002  
马欢 河南省农业科学院 农业质量标准与检测技术研究所/河南省粮食质量安全与检测重点实验室/农业部农产品质量安全风险评估实验室(郑州), 郑州 450002  
安莉 河南省农业科学院 农业质量标准与检测技术研究所/河南省粮食质量安全与检测重点实验室/农业部农产品质量安全风险评估实验室(郑州), 郑州 450002  
吴家锴 河南省农业科学院 农业质量标准与检测技术研究所/河南省粮食质量安全与检测重点实验室/农业部农产品质量安全风险评估实验室(郑州), 郑州 450002  
汪红 河南省农业科学院 农业质量标准与检测技术研究所/河南省粮食质量安全与检测重点实验室/农业部农产品质量安全风险评估实验室(郑州), 郑州 450002  
祁玉峰 河南省农业科学院 农业质量标准与检测技术研究所/河南省粮食质量安全与检测重点实验室/农业部农产品质量安全风险评估实验室(郑州), 郑州 450002  
陈寅 河南省粮食科学研究所有限公司, 郑州 450008  
吴绪金 河南省农业科学院 农业质量标准与检测技术研究所/河南省粮食质量安全与检测重点实验室/农业部农产品质量安全风险评估实验室(郑州), 郑州 450002 xujinwu2005@126.com 
基金项目:粮油作物产品未知危害因子识别与已知危害因子安全性评估项目(GJFP2015007);河南省农业科学院基础科研项目(2016)
中文摘要:采用QuEChERS样品前处理方法,建立了主要谷物和油料作物产品(糙米、小麦、玉米和大豆)中氯虫苯甲酰胺残留量的高效液相色谱-串联质谱(HPLC-MS/MS)检测方法。样品经乙腈-水提取及盐析处理后,用N-丙基乙二胺(PSA)和石墨化碳黑(GCB)固相萃取填料净化,高效液相色谱-串联质谱(HPLC-MS/MS)、多反应监测模式(MRM)下测定。基质标准曲线外标法定量。结果表明:在0.005~0.5 mg/L范围内,不同样品基质中氯虫苯甲酰胺的峰面积与其相应的质量浓度间均有良好的线性关系(R2>0.99),检出限(LOD)为0.001 mg/L。在0.02、0.05、0.1和0.5 mg/kg添加水平下,氯虫苯甲酰胺在4种基质中的平均回收率在89%~114%之间,相对标准偏差(RSD)在1.3%~11%(n = 5)之间,4种基质中的最低检测浓度(LOQ)均为0.02 mg/kg。该方法适用于主要谷物和油料作物产品中氯虫苯甲酰胺残留量的检测。
中文关键词:QuEChERS  高效液相色谱-串联质谱  氯虫苯甲酰胺  谷物  油料作物  残留
 
QuEChERS-determination of chlorantraniliprole residues in primary grain and oilseed crops by high performance liquid chromatography-tandem mass spectrometry
Abstract:A rapid, simple and efficient analytical method for the determination of chlorantraniliprole in different primary grain and oilseed crops including brown rice, wheat, maize and soybean was developed and validated based on QuEChERS and high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Chlorantraniliprole residues were extracted from primary grain and oilseed crops samples using acetonitrile-water with the addition of sodium chloride. After centrifugation, the upper solvent was cleaned-up by N-propylethyl-diamine (PSA) and graphitizing of carbon black (GCB), and determined by HPLC-MS/MS under multiple reaction monitoring mode (MRM). Sample matrix-matched calibrations were used to determine the residue contents by external standard. The calibration curves showed a good linearity in the concentration range of 0.005-0.5 mg/L for chlorantraniliprole in different sample matrix. The determination coefficients (R2) of the calibration curves were all above 0.99 and the limit of detection (LOD) was 0.001 mg/L. At fortification levels of 0.02, 0.05, 0.1 and 0.5 mg/kg in different primary grain and oilseed crop samples, recoveries ranged from 89% to 114% with relative standard deviation (RSD) of 1.3% to 11% (n = 5). The limit of quantification (LOQ) of chlorantraniliprole in brown rice, wheat, maize and soybean were all 0.02 mg/kg. This new method is applicable to detect the residues of chlorantraniliprole in different primary grain and oilseed crops.
Key words:QuEChERS  high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS)  chlorantraniliprole  grain  oilseed crops  residue
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