| 节梦蕾,时英爽,高有华,韩瑶,袁震,景伟文.基质分散固相萃取-QuEChERS耦合HPLC法测定棉花叶片中吡虫啉及其相关代谢物[J].干旱地区农业研究,2020,38(6):249~254 |
| 基质分散固相萃取-QuEChERS耦合HPLC法测定棉花叶片中吡虫啉及其相关代谢物 |
| 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 |
| 中文关键词: 吡虫啉 代谢物 棉花叶片 QuEChERS方法 |
| 英文关键词:imidacloprid metabolites cotton leaves QuEChERS pretreatment method |
| 基金项目:国家重点研发计划项目(2016YFD0200207-3)；新疆农业大学大学生创新基金 |
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| 中文摘要: |
| 建立了QuEChERS前处理的棉花叶片中吡虫啉及其代谢物含量的高效液相色谱（HPLC）分析方法。在QuEChERS前处理方法的基础上，确定了乙腈作为提取剂，盐析材料为1.00 g氯化钠、4.00 g无水硫酸镁、0.50 g柠檬酸二钠和1.00 g柠檬酸钠，净化材料为25 mg的N-丙基乙二胺（PSA），在2%乙腈-甲醇∶水=3∶7条件下HPLC法进行定量测定。结果表明：棉花叶片中的吡虫啉及其4种代谢物吡虫啉脲、烯式吡虫啉、吡虫啉胍和6-氯烟酸的平均加标回收率为92.84%~110.90%，相对标准偏差（RSD）在0.15%~6.99%之间，检出限（LOD）分别为0.0044、0.042、0.0011、0.091 mg·kg-1和0.0066 mg·kg-1，定量限（LOQ）分别为0.015、0.19、0.0059、0.036 mg·kg-1和0.028 mg·kg-1。该分析方法前处理简便、快速、准确，可为棉花叶片中吡虫啉及其代谢物残留的测定提供参考。 |
| 英文摘要: |
| 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. |
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