N-乙烯吡咯烷酮-二乙烯苯的磺化改性及其在柑橘农残检测中的应用  

Sulfonation modification of N-vinylpyrrolidone-divinylbenzene and its application to the detection of pesticide residues in citrus

作　　者：张舜光 何柳 赵相相 袁开怀 张欢[1] ZHANG Shunguang;HE Liu;ZHAO Xiangxiang;YUAN Kaihuai;ZHANG Huan(School of Chemistry and Chemical Engineering,Tianjin University of Technology,Tianjin 300384,China;Cecep Runda(Yantai)Environmental Protection Company Limited,Yantai 264006,China)

机构地区：[1]天津理工大学化学化工学院,天津300384 [2]中节能(烟台)润达环保股份有限公司,烟台264006

出　　处：《分析试验室》2025年第4期479-486,共8页Chinese Journal of Analysis Laboratory

基　　金：国家自然科学基金(22203063)资助。

摘　　要：对固相萃取(SPE)填料N-乙烯吡咯烷酮-二乙烯苯(NVP-DVB)进行磺化修饰,得到非极性吸附/阳离子交换型填料NVP-DVB-S,与高效液相色谱法结合用于检测柑橘中吡虫啉、苯菌灵、噻菌灵和多菌灵的残留。优化的磺化反应条件为:反应时间8 h,反应温度80℃,磺化剂用量NVP-DVB∶H_(2)SO_(4)(m/m)=1∶5。采用扫描电子显微镜(SEM)、比表面积与孔隙度分析(BET)和元素分析对制备的系列填料进行表征,系列填料平均孔径范围为5.77~7.38 nm,比表面积范围为457.59~620.25 m^(2)/g,孔容范围为0.98~1.25 cm^(3)/g。对制备的系列填料进行SPE应用,被测的4种药品在0.075~5.0μg/m L浓度范围内与色谱峰面积有良好的线性关系,相关系数在0.9993~0.9999之间,检出限为0.29~0.56μg/L。对不同硫含量的NVP-DVB-S进行回收实验,结果表明:硫含量为5.14%时,可用于柑橘中4种药品的同时检测;硫含量在2.33%时,对多菌灵和噻菌灵的吸收效果更好;硫含量为6.43%时,对吡虫啉的回收性能较好。The solid phase extraction(SPE)filler of N-vinylpyrrolidone-divinylbenzene(NVP-DVB)was sulfonated and modified to obtain the nonpolar adsorption/cation-exchange filler of NVP-DVB-S,which was combined with highperformance liquid chromatography(HPLC)to determine imidacloprid,benomyl,thiabendazole and carbendazim residues in citrus.The optimum sulfonation reaction conditions were as follows:reaction time of 8 h,reaction temperature of 80℃,and sulfonating agent dosage of NVP-DVB∶H_(2)SO_(4)(m/m)=1∶5.The prepared fillers series were characterized using scanning electron microscope(SEM),BET and elemental analysis.The average pore sizes of the fillers prepared were 5.77?7.38 nm,the specific surface area ranged from 457.59 to 620.25 m^(2)/g,and the pore volume ranged from 0.98 to 1.25 cm^(3)/g.By using NVP-DVB-S series as filler for SPE of target pesticide residues,the four drugs tested showed good linearity in the concentration range of 0.075?5.0μg/m L,with the detection limits of 0.29?0.56μg/L and the correlation coefficients of 0.9993?0.9999.Recovery experiments were carried out by using NVP-DVB-S with different sulfur contents for SPE.The results showed that the NVP-DVB-S with sulfur content of 5.14%could be used for the simultaneous detection of four drugs in citrus;the NVP-DVB-S with the sulfur content of 2.33%showed better absorption performance for carbendazim and thiabendazole;and the NVP-DVB-S with sulfur content of 6.43%showed a better recovery performance for imidacloprid.

关 键 词：磺化 功能材料 固相萃取 高效液相色谱法 

分 类 号：O625.6[理学—有机化学]