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目的建立QuEChERS-高效液相色谱串联质谱法(QuEChERS-high performance liquid chromatography tandem mass spectrometry)检测豆芽与其生产环境水样中多菌灵的痕量残留分析方法,并对豆芽中多菌灵残留降解和测量不确定度的各因素进行分析。方法样品用0.1%乙酸乙腈提取,经QuEChERS净化,液相色谱-串联质谱测定,外标法定量。结果本方法在10.0~200.0μg/L范围内的线性关系良好(r~2>0.999),空白豆芽中分别添加50、100、200μg/kg 3个质量浓度水平,平均回收率为85.7%~93.6%,相对标准偏差为2.02%~5.19%,方法的检出限(LOD)为16μg/kg;空白水样中分别添加0.05、0.10、0.20μg/kg 3个浓度水平,平均回收率为84.2%~90.4%,相对标准偏差为3.84%~5.53%,方法的检出限(LOD)为0.02μg/kg。多菌灵残留降解的处理浓度对其残留量的影响大于采收日期、温度处理和喷水处理;测定结果的不确定度主要来源于回收率、采用最小二乘法拟合标准工作曲线求得样品浓度过程及标准溶液的配制。结论本研究方法的LOD较低,前处理简单、快速,灵敏度及准确度均符合农药残留检测要求,适用于豆芽和水样中的多菌灵痕量残留分析。
OBJECTIVE To establish a method for the determination of carbendazim and carbendazim in water samples of its production by QuEChERS-high performance liquid chromatography tandem mass spectrometry (GC-MS / MS), and analyze the residues of carbendazim in bean sprout The factors that determine the uncertainty are analyzed. Methods The samples were extracted with 0.1% acetic acid, purified by QuEChERS, determined by liquid chromatography-tandem mass spectrometry and quantified by external standard method. Results The linearity was good in the range of 10.0 ~ 200.0μg / L (r ~ 2> 0.999). The blank bean sprouts were respectively treated with 50, 100 and 200μg / kg of 3 mass concentration with the average recoveries of 85.7% ~ 93.6 %, And the relative standard deviations were 2.02% -5.19%. The detection limit (LOD) of the method was 16μg / kg. The blank water samples were respectively treated with three concentration levels of 0.05, 0.10 and 0.20μg / kg with the average recovery of 84.2% ~ 90.4%, and the relative standard deviation was 3.84% ~ 5.53%. The limit of detection (LOD) was 0.02 μg / kg. The effect of carbendazim residue degradation on its residual amount was greater than that on harvest date, temperature treatment and water spray treatment. The uncertainty of the determination results mainly came from the recovery rate. The least square method was used to fit the standard working curve to obtain the sample Concentration process and standard solution preparation. Conclusion The method has low LOD, simple pretreatment, fastness, sensitivity and accuracy to meet the requirements of pesticide residue detection. It is suitable for the analysis of trace levels of carbendazim in bean sprouts and water samples.