摘要
[目的]建立超高效液相色谱-串联质谱法(UPLC-MS/MS),测定茶叶中呋虫胺及其代谢物1-甲基-3-[(3-四氢呋喃)甲基]二氢胍盐(DN)、1-甲基-3-[(3-四氢呋喃)甲基]脲(UF)和唑虫酰胺残留量,并研究其低温储藏稳定性。[方法]样品经改进后的QuEChERS方法提取净化,采用0.1%甲酸水溶液-0.1%甲酸乙腈为流动相洗脱,电喷雾(ESI)、多反应监测(MRM)正离子扫描,基质配标外标法定量,分别研究样品储藏、模拟运输、提取液中的残留量变化。[结果]在0.05、1.0、20、50 mg/kg添加水平下,呋虫胺及其代谢物和唑虫酰胺在茶叶中的平均回收率为84%~102%,相对标准偏差(RSDs)为1%~7%,定量限为0.05 mg/kg。在<-18℃储藏条件、<4℃模拟运输、20℃提取液存放过程中,目标化合物降解率均低于30%。[结论]方法精确度满足残留检测要求,可同时分析茶叶中呋虫胺及其代谢物和唑虫酰胺的残留量,在<-18℃储藏条件下,目标化合物的储藏稳定期为199 d,低于4℃在72 h内运输是稳定的,提取液在49 h内完成检测可保证数据准确性。
[Aims] The aim is to establish a UPLC-MS/MS method to measure residues of dinotefuran, its metabolites1-methyl-3-[(3-tetrahydrofuran)methyl]dihydroguanidine(DN) and 1-methyl-3-[(3-tetrahydrofuran)methyl]urea(UF),and tolfenpyrad in tea, and to investigate the storage stability of these compounds at low temperature. [Methods] The samples were extracted and purified by the modified QuEChERS method. The 0.1% formic acid aqueous solution-0.1% formic acid acetonitrile was used as mobile phase. The positive ion scanning mode was set in ESI and MRM.The external standard method was used for quantitative analysis. The sample storage, simulated transportation and sample extract were studied for the changes of residual amount, respectively. [Results] At the addition levels of0.05, 1.0, 20 and 50 mg/kg, the average recovery rates of dinotefuran and its metabolites and tolfenpyrad in tea were 84%-102%, with relative standard deviations(RSDs) of 1%-7% and a quantification limit of 0.05 mg/kg.During storage conditions below-18 ℃, simulated transportation below 4 ℃, and storage of extraction solution at20 ℃, the degradation rates of the target compounds were all below 30%. [Conclusions] The accuracy of the method meets the requirements of residue detection. The residues of dinotefuran and its metabolites and tolfenpyrad could be simultaneously analyzed in tea. The storage stability period of the target compounds is 199 d under storage conditions below-18 ℃. The target compounds are stable when transported within 72 h below 4 ℃. In addition, the extraction solution detected within 49 h can ensure the accuracy of the data.
作者
王彬
李春勇
吕莹
秦曙
WANG Bin;LI Chunyong;LYUYing;QIN Shu(Shanxi Center for Testing of Functional Agro-Products,Shanxi Agricultural University,Taiyuan 030031,China)
出处
《农药》
北大核心
2025年第2期119-125,共7页
Agrochemicals
基金
山西省高等学校科技创新项目(2022L079)。
