Determination of imidacloprid and its metabolites in cotton leaves by HPLC coupled with matrix solid\|phase dispersion\|QuEChERS methods
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DOI:10.7606/j.issn.1000-7601.2020.06.33
Key Words: imidacloprid  metabolites  cotton leaves  QuEChERS pretreatment method
Author NameAffiliation
IE Menglei ollege of Chemical Engineering, Xinjiang Agricultural University, Urumqi, Xinjiang 830052, China 
SHI Yingshuang ollege of Chemical Engineering, Xinjiang Agricultural University, Urumqi, Xinjiang 830052, China 
GAO Youhua College of Agriculture, Xinjiang Agricultural University, Urumqi, Xinjiang 830052, China 
HAN Yao ollege of Chemical Engineering, Xinjiang Agricultural University, Urumqi, Xinjiang 830052, China 
YUAN Zhen ollege of Chemical Engineering, Xinjiang Agricultural University, Urumqi, Xinjiang 830052, China 
JING Weiwen ollege of Chemical Engineering, Xinjiang Agricultural University, Urumqi, Xinjiang 830052, China 
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Abstract:
      This paper aimed to establish a method for determining imidacloprid and its metabolite residues in cotton leaves by high performance liquid chromatography coupled with QuEChERS pretreatment methods. Based on QuEChERS method, acetonitrile was used as the extraction agent and 1.00 g of sodium chloride, 4.00 g of anhydrous magnesium sulfate, 0.50 g of disodium citrate and 1.00 g of sodium citrate were applied as the salting\|out agent. 25 mg of PSA sorbent was selected as the purification agent and the mixture of 2% acetonitrile\|methanol and water with the proportion of 3∶7 was used as the mobile phase. The results showed that the average spiked recoveries of imidacloprid and its four metabolites (imidacloprid urea, olefin imidacloprid, guanidine\|imidacloprid, and 6-chloronicotinic acid) were in the range of 92.84%~110.90% and the relative standard deviation (RSD) were 0.15%~6.99% in cotton leaves. The detection limits (LOD) were 0.0044, 0.042, 0.0011, 0.091 mg·kg-1, and 0.0066 mg·kg-1, respectively, and the limits of quantitation (LOQ) were 0.015, 0.19, 0.0059, 0.036 mg·kg-1, and 0.028 mg·kg-1, respectively. The method was had simple, rapid, and precise pretreatment and could provide reference for the determination of imidacloprid and its metabolite residues in cotton leaves.