QuEChERS-高效液相色谱串联质谱法测定豆芽与生产环境水样中多菌灵残留及其不确定度评估

Determination and uncertainty analysis of carbendazim residues in bean sprout and its contaminate water sources by QuEChERS and high performance liquid chromatography tandem mass spectrometry

中文关键词:  多菌灵  QuEChERS-液相色谱-串联质谱  豆芽  水  不确定度

英文关键词:carbendazim  QuEChERS and high performance liquid chromatography tandem mass spectrometry  bean sprouts  water  uncertainty

中文摘要:

      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10.0~200.0 μg/L范围内的线性关系良好(r2>0.999), 空白豆芽中分别添加50、100、200 μg/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16 μg/kg; 空白水样中分别添加0.05、0.10、0.20 μg/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0.02 μg/ 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。

英文摘要:

      Objective To establish a method for trace level analysis of carbendazim in bean-sprout and its contaminate sources water by QuEChERS and high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS). The degradation of carbendazim in bean sprout and the uncertainty originated from the measurement of carbendazim in bean sprout were analyzed and evaluated. Methods The sample was extracted with 0.1% acetic acid acetonitrile directly, and purified by QuEChERS, then analyzed by HPLC-MS/MS. The quantization was carried out by the external standard method. Results A good linear relationship was obtained in the range of 10~200.0 μg/L with the correlation coefficient (r2) over 0.999. The recoveries of carbendazim in blank bean sprout at 3 spiked levels of 50, 100, 200 μg/kg ranged from 85.7%~93.6%, the relative standard deviation (RSD) from 2.02%~5.19%, and the limit of detection (LOD) of the method was 16 μg/kg. The recoveries of carbendazim in blank water at 3 spiked levels of 0.05, 0.10, 0.20 μg/kg ranged from 84.2%~90.4%, the RSD from 3.84%~5.53%, and the LOD of the method was 0.02 μg/kg. The impact of the processing concentration on the residues was greater than the harvest time, processing temperature and spray water. The measurement uncertainty was mainly due to recovery rate, the least square fitting of the working curve and preparation process of standard solution. Conclusion This method is simple, rapid and characterized with acceptable sensitivity and accuracy to meet the requirements of the carbendazim residue analysis, which is suitable for the conformation and quantification of the carbendazim in bean sprout and its contaminate water sources.