摘要
[目的]建立超高效液相色谱-串联质谱法测定不同环境介质中的溴虫氟苯双酰胺及其代谢物(DC-8007)的分析方法。[方法]水样采用酸化乙腈提取,土壤和沉积物样品采用乙腈-0.5 mol/L HCl水溶液(体积比1∶1)提取,PSA净化后,利用超高效液相色谱-串联质谱仪(UPLC-MS/MS)在多反应离子扫描模式(MRM)下进行检测。[结果]溴虫氟苯双酰胺及其代谢物DC-8007在0.0001~0.05 mg/L质量浓度范围内线性关系良好(R^(2)>0.995),水样添加质量浓度为0.0002~0.01 mg/L,土壤和沉积物添加质量分数为0.001~0.05 mg/kg时,其平均回收率为76.9%~95.1%,相对标准偏差为1.7%~8.5%;水中定量限为0.0002 mg/L,土壤和沉积物中定量限为0.001 mg/kg。[结论]该方法简单快速、灵敏度高、重现性好,适用于不同环境介质中溴虫氟苯双酰胺及其代谢物的测定。
[Aims]The study aimed to establish the analysis method for the determination of broflanilide and its metabolite(DC-8007)in different matrix by UPLC-MS/MS.[Methods]The water samples were extracted by acidified acetonitrile,while the soil and sediments were firstly extracted with acetonitrile-0.5 mol/L HCl aqueous solution(1:1,by vol)and purified with PSA,then determined by ultra performance liquid chromatography-mass spectrometry under multiple reaction monitoring.[Results]There was a good linear relationship between the concentration of broflanilide as well as its metabolite and the peak area in the range of 0.0001-0.05 mg/L(R>0.995).The average recoveries of broflanilide and DC-8007 were 76.9%-95.1%,while the RSD values were 1.7%-8.5%,at the spiked levels of 0.001,0.01,0.05 mg/kg in soil or 0.0002,0.002,0.01 mg/L in water.The quantification limit of the broflanilide and DC-8007 was 0.0002 mg/L in water and 0.001 mg/kg in soil and sediments.[Conclusions]The method is simple with high accuracy and precision,which is suitable for simultaneous determination of broflanilide and its metabolite in different matrix.
作者
曹莉
许静
宋宁慧
豆叶枝
李菊颖
余佳
何健
张悦清
吴文铸
孔德洋
CAO Li;XU Jing;SONG Ning-hui;DOU Ye-zhi;LI Ju-ying;YU Jia;HE Jian;ZHANG Yue-qing;WU Wen-zhu;KONG De-yang(Nanjing Institute of Environmental Sciences,Ministry of Ecology and Environment of the People's Republic of China,Key Laboratory of Pesticide Environmental Assessment and Pollution Control,Ministry of Environmental Protection,Nanjing 210042,China)
出处
《农药》
CAS
CSCD
北大核心
2023年第6期448-452,共5页
Agrochemicals
基金
中央级公益性科研院所基本科研业务费重点项目“基于高分辨质谱高通量识别的污染精准溯源技术研究及应用”(GYZX230104)
国家重点研发计划“国家生态环境保护与风险防控标准体系与关键标准研制”子课题(SQ2020YFC1806300-08)。
