摘要
目的建立QuEChERs-超高效液相色谱三重四级杆线性离子阱串联质谱法测定果蔬中64种农药的残留量。方法通过优化传统的QuEChERS前处理方法,解决了传统QuEChERS法中前处理试样结块、农药回收率偏低及重现性差的问题;采用超高效液相色谱三重四级杆线性离子阱串联质谱法对果蔬中64种农残进行检测,通过增加切换阀步骤,减少质谱仪不必要的污染,保护质谱系统。结果仪器在10.00min之内完成64种目标物的定量测定。使用外标法绘制64种农药的校准曲线,线性良好,相关系数绝大部分在0.9990以上。方法检出限低,可用于对痕量农药残留的检测。对64农药进行不同基质的加标回收实验,回收率在70%～111%之间。结论该方法前处理简便,分析速度快、灵敏度高,适合于蔬菜、水果中多种残留物的初筛、痕量检测和定量检测分析。
Objective To establish a method for the determination of 64 pesticide residues in fruits and vegetables by QuEChERs-ultra performance liquid chromatography triple quadruple-rod linear ion trap tandem mass spectrometry. Methods The problems of sample agglomeration, low pesticide recovery and poor reproducibility in the traditional QuEChERS pretreatment method were solved by optimizing the traditional QuEChERS pretreatment method. Totally 64 kinds of pesticide residues in fruits and vegetables were detected by ultra performance liquid chromatography triple four-pole linear ion trap tandem mass spectrometry, and unnecessary pollution of mass spectrometer was reduced by adding switching valve steps, and mass spectrometry system was protected. Results Quantitative determination of 64 target substances was completed within 10.00 min. The calibration curves of 64 pesticides were plotted by external standard method, and the linearity was good. Most of the correlation coefficients were above 0.9990. The method had low detection limit and could be used for the detection of trace pesticide residues. A total of 64 pesticides were recovered with different substrates, and the recoveries ranged from 70% to111%. Conclusion The method is simple, rapid and sensitive, which is suitable for the preliminary screening, trace detection and quantitative analysis of various residues in vegetables and fruits.
引文
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