超高效液相色谱-串联质谱法测定果蔬中新烟碱类农药残留

Determination of neonicotinoid insecticides in fruits and vegetables by ultra-high performance liquid chromatography-tandem mass spectrometry

目的建立水果蔬菜中12种新烟碱类农药(吡虫啉、啶虫脒、噻虫啉、噻虫嗪、噻虫胺、呋虫胺、烯啶虫胺、氯噻啉、哌虫啶、环氧虫啶、氟啶虫胺腈、氟吡呋喃酮)残留量的超高效液相色谱-质谱联用测定方法。在黑龙江省范围内采集水果蔬菜样品进行检测,分析数据,并根据监测风险提示,给出建设性措施和建议。方法样品用乙腈提取,采用QuEChERS(quick,easy,cheap,effective,rugged,safty)前处理技术,提取液经分散固相萃取净化,超高效液相色谱-质谱联用仪测定,正离子源(electrospray ionization,ESI+)多反应监测(multiple response monitoring,MRM)模式下检测,外标法定量并进行结果分析,实现了同时测定果蔬中12种烟碱类农药的残留量。结果12种烟碱类农药线性范围为5~200 ng/mL,相关系数均>0.999。检出限为0.001 mg/kg,定量限为0.005 mg/kg。在加标水平为5、50、200 ng/mL时,平均加标回收率为89.8%~113.9%,相对标准偏差为0.4%~3.4%。黑龙江省采样341份样本,检出107件,检出率31.4%。结论该方法操作简单、快速、准确度和灵敏度高,可以做到批量测定,具有良好的实际应用前景。

Objective To establish an ultra-high performance liquid chromatography-mass spectrometry(UPLC-MS/MS)method for the determination of residues of 12 neonicotinoid insecticides(imidacloprid,acetamiprid,thiamethoprid,thiamethoxam,thiamethoxam,clothianidin,dinotefuran,nitenpyram,imidaclothiz,IPP,cycloxaprid,sulfoxaflor,flufuranone)in fruits and vegetables.Collect fruit and vegetable samples within Heilongjiang Province for testing,analyze data,and give constructive measures and suggestionsac-cording to the monitoring risk tips.Methods The samples were extracted with acetonitrile,purified by dispersive solid phase extraction using quick,easy,cheap,effective,rugged,safty(QuEChERS)pretreatment technique,determined by ultra-high performance liquid chromatography-mass spectrometry,detected by electrospray ionization(ESI+)multiple reaction monitoring(MRM)mode,quantified by external standard method and the results were analyzed,achieving simultaneous determination of residues of 12 neonicotinoid insecticides in fruits and vegetables.Results The linear ranges of 12 neonicotinoid insecticides were 5-200 ng/mL,with all the correlation coefficients>0.999.The limits of detection was 0.001 mg/kg,and the limits of quantification was 0.005 mg/kg.Atspiked levels of 5,50 and 200 ng/mL,the average recoveries of the method ranged from 89.8%to 113.9%,with a relative standard deviation of 0.4%to 3.4%.Totally 107 samples were detected from 341 samples,with a detection rate of 31.4%.Conclusion The method is simple,rapid,accurate and sensitive.It can be used in batch measurement and has a good practical application prospect.