Accurate Quantification of Pure Thiacloprid with Mass Balance and Quantitative H-NMR  

作　　者：Mengling Tu Wei Zhang Yunxiao Zhu Wen Ma Xiao Li Shukun Zhou Hongmei Li Xianjiang Li 

机构地区：[1]Key Laboratory of Chemical Metrology and Applications on Nutrition and Health for State Market Regulation,Division of Metrology in Chemistry,National Institute of Metrology,Beijing 100029,China [2]State Key Laboratory of Heavy Oil Processing,College of Chemical Engineering and Environment,China University of Petroleum,Beijing 102249,China [3]State Key Laboratory of Natural and Biomimetic Drugs,School of Pharmaceutical Sciences,Peking University,Beijing 100191,China

出　　处：《Journal of Analysis and Testing》2024年第1期1-8,共8页分析检测（英文）

基　　金：financially supported by the State Administration for Market Regulation(QNBJ202306);the National Natural Science Foundation of China(22004004).

摘　　要：Thiacloprid is the first-generation neonicotinoid insecticide,which is widely used in modern agriculture.Reference materials are essential for sound measurement and traceability of results in chemical analysis.Pure thiacloprid was comprehensively assessed by two orthonormal methods:mass balance(MB) and quantitative nuclear magnetic resonance spectroscopy(qNMR).From MB,its mass fraction value was 998.4 mg/g with the subtraction of structurally related impurities(99.87%),inorganic impurities(0.006 mg/g),water(0.33 mg/g),and volatile organic solvent(0 mg/g).To guarantee sufficient separation of structurally related purity,peak purity of thiacloprid was evaluated by five points of UV spectra.From the qNMR of hydrogen,its mass fraction value was 995.7 mg/g which was traced to the internal standard(methyl sulfone).Finally,the certified value was assigned to 997 mg/g,together with an expanded uncertainty of 3 mg/g(k=2).This high-purity thiacloprid can be applied to routine monitoring in agriculture and the food fields.

关 键 词：Mass balance Quantitative nuclear magnetic resonance spectroscopy Reference material THIACLOPRID 

分 类 号：TQ450.7[化学工程—农药化工] O657.61[理学—分析化学]