论文部分内容阅读
目的建立应用气相色谱质谱/质谱法(gas chromatography/mass spectrograph/mass spectrograph,GC/MS/MS)同时测定茶叶中茚虫威、溴虫腈和啶虫脒的方法。方法收集吉林省10个市的210份茶叶样品,样品经乙腈提取,氮吹浓缩,固相萃取柱净化,浓缩定容后,采用三重四级杆气质联用仪,MRM测定,对质谱测定的目标离子对进行选择。结果茚虫威、溴虫腈、啶虫脒的质量浓度在0.05~1.0μg/m L范围时,其峰面积与浓度间呈现良好的线性关系,方法的检出限和定量限分别为0.01 mg/kg和0.03 mg/kg,3种农药在3个添加水平下的平均加标回收率为84%~110%,相对标准偏差(relative standard deviation,RSD)≤10.12%。样品中茚虫威的超标率为2.86%,啶虫脒的超标率高达22.86%。结论 GC/MS/MS法的精密度和准确度较好,能够实现茶叶样品中茚虫威、溴虫腈和啶虫脒的同时准确测定。
Objective To establish a method for simultaneous determination of indoxacarb, chlorfenapyr and acetamiprid in tea by gas chromatography / mass spectrometry / mass spectrometry (GC / MS / MS). Methods A total of 210 samples of tea from 10 cities of Jilin Province were collected. The samples were extracted with acetonitrile, concentrated by nitrogen and purified by solid phase extraction (SPE). The contents of the samples were concentrated and quantified by triple quadrupole mass spectrometry (MRS) The target ion pair is selected. Results The linear range of peak area and concentration of indoxacarb, chlorfenapyr and acetamiprid in the concentration range of 0.05-1.0 μg / mL was linear with the limits of detection (LOQ) and limit of quantification (LOQ) of 0.01 mg / kg and 0.03 mg / kg respectively. The average recovery of three pesticides was 84% -110% with relative standard deviation (RSD) ≤10.12%. In the sample indoxacarb exceeded the rate of 2.86%, acetamiprid exceeded the rate of up to 22.86%. Conclusion The precision and accuracy of GC / MS / MS method are good, and the simultaneous and accurate determination of indoxacarb, chlorfenapyr and acetamiprid in tea samples can be achieved.