摘要
建立了QuEChERS净化结合气相色谱串联质谱测定诺丽酵素原液中12种农药残留的方法。样品采用乙腈溶液提取,提取液中加入无水硫酸镁、氯化钠、柠檬酸钠、柠檬酸氢二钠脱水和缓冲,振荡分层后吸取上层清液,再经PSA净化离心后上机。结果表明,50 mg PSA能够满足方法的净化要求,12种农药均采用外标法定量,基质标准溶液在0.005~0.960 mg/L线性良好;在0.012、0.080、0.400 mg/kg 3个添加水平下回收率为84.2%~113.0%,RSD均小于15%,大部分农药定量限为0.012 mg/kg。该方法前处理简单快速,准确度和精密度符合检测要求,可满足诺丽酵素原液中的乙烯菌核利、腐霉利、联苯菊酯等12种农药残留的同时检测。
A method has been developed for the simultaneous determination of 12 pesticides residues in fermentation broth of Morinda citrifolia using QuEChERS-gas chromatography-tandem mass spectrometry.The residue of 12 pesticides were extracted from samples by acetonitrile,then the extracting solution was cleaned up with PSA.Finally,the pesticides was analysed by gas chromatography-mass spectrometry under MRM mode via electrospray ionization.All pesticides were quantified by external standard method.The matrix calibration curves of the pesticides were linear in the range of 0.005~0.960 mg/L.The average recoveries of target compounds at three spiked concentration levels of 0.012,0.08,0.40 mg/kg were in the range of 84.2%~113.0%,RSD were less than 15%,the limit of quantification of most pesticides were 0.012 mg/kg.The results demonstrated the method is simple,fast aaccurated and can be used for analysis of the multiclass of pesticide residues in fermentation broth of morinda citrifolia.
作者
吴南村
张群
刘春华
马晨
吴学进
WU Nan-cun;ZHANG Qun;LIU Chun-hua;MA Chen;WU Xue-jin(Analysis and Testing Center,Chinese Academy of Tropical Agricultural Sciences,Haikou 571101,China;Hainan Key Laboratory for Quality and Safety of Tropical Fruits and Vegetables,Haikou 571101,China)
出处
《湖北农业科学》
2019年第1期96-99,共4页
Hubei Agricultural Sciences
基金
海南省自然科学基金项目(317226)
中国热带农业科学院基本科研业务费专项(1600082016003
1600082017003)