Determination of Residues of 4 Fungicides in Fruit Juice by High Performance Liquid Chromatography with Dispersion Solid Phase Extraction Based on Magnetic Carbon Nanotubes Modified with Deep Eutectic Solvent
摘 要
提出了基于低共熔溶剂(DES)修饰磁性碳纳米管的分散固相萃取-高效液相色谱法测定4种杀菌剂残留量的方法。将氯化胆碱与乙二醇按物质的量比1∶2混合,用磁力搅拌器涡旋加热直到获得透明的DES,再用2 mL DES和0.4 g磁性碳纳米管制备DES修饰磁性碳纳米管。取5 mL水置于离心管中,加入200 μL果汁样品和16 mg DES修饰磁性碳纳米管,超声提取10 min,在外加磁场作用下沉淀30 min,去除上层液体,再加入1 mL乙醇,涡旋2.5 min,过0.22 μm滤膜,采用高效液相色谱法测定滤液中异菌脲、氯苯嘧啶醇、腈菌唑、醚菌酯等4种杀菌剂的含量。结果表明,4种杀菌剂的质量浓度在0.5~5.0 mg·L-1内与对应的峰面积呈线性关系,检出限(3S/N)依次为0.04,0.11,0.15,0.16 mg·L-1。按照标准加入法进行回收试验,回收率为81.5%~98.9%,测定值的相对标准偏差(n=6)均小于7.0%。
Abstract
A method for the determination of residues of 4 fungicides by high performance liquid chromatography (HPLC) with dispersion solid phase extraction based on magnetic carbon nanotubes modified with deep eutectic solvent (DES) was proposed. Choline chloride and glycol were mixed at the molar ratio of 1∶2, which was heated by vortex with a magnetic agitator until the transparent DES was obtained. Magnetic carbon nanotubes modified with DES were prepared with 2 mL of DES and 0.4 g of magnetic carbon nanotubes. 5 mL of water was taken and placed in a centrifuge tube, and 200 μL of fruit juice sample and 16 mg of magnetic carbon nanotubes modified with DES were added. The mixture was extracted by ultrasound for 10 min and precipitated for 30 min under external magnetic field. The upper liquid was removed and 1 mL of ethanol was added. After vortex for 2.5 min, the mixture was passed through a 0.22 μm filter membrane. Four fungicides, including iprodione, fenarimol, myclobutanil, and kresoxim-methyl, in the filtrate were determined by HPLC. As shown by the results, linear relationships between values of mass concentration of 4 fungicides and the corresponding peak area were found in the range of 0.5-5.0 mg·L-1, with detection limits (3S/N) of 0.04 mg·L-1 for iprodione, 0.11 mg·L-1 for fenarimol, 0.15 mg·L-1 for myclobutanil and 0.16 mg·L-1 for kresoxim-methyl, respectively. Test for recovery was made by the standard addition method, giving results in the range of 81.5%-98.9%, with RSDs (n=6) of the determined values less than 7.0%.
中图分类号 O657.7 DOI 10.11973/lhjy-hx202306004
所属栏目 工作简报
基金项目 河北省教育厅青年基金研究项目(QN2022030);河北省农产品食品质量安全分析检测重点实验室项目(AFS202101);河北省科技厅技术创新项目(V1623806634552)
收稿日期 2022/5/7
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备注庚丽丽,讲师,硕士,主要从事功能材料合成及农产品分析检测
引用该论文: GENG Lili,SUN Haifu,HU Xiaoling,ZHANG Yanan,CANG Bohang,WANG Suli. Determination of Residues of 4 Fungicides in Fruit Juice by High Performance Liquid Chromatography with Dispersion Solid Phase Extraction Based on Magnetic Carbon Nanotubes Modified with Deep Eutectic Solvent[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2023, 59(6): 643~648
庚丽丽,孙海富,胡晓玲,张亚南,苍博杭,王素利. 基于低共熔溶剂修饰磁性碳纳米管的分散固相萃取-高效液相色谱法测定果汁中4种杀菌剂的残留量[J]. 理化检验-化学分册, 2023, 59(6): 643~648
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参考文献
【1】WANG A Z, MAHAI G G, WAN Y J, et al. Neonicotinoids and carbendazim in indoor dust from three cities in China: Spatial and temporal variations[J]. The Science of the Total Environment, 2019,695:133790.
【2】CHAWLA P, KAUSHIK R, SHIVA SWARAJ V J, et al. Organophosphorus pesticides residues in food and their colorimetric detection[J]. Environmental Nanotechnology, Monitoring & Management, 2018,10:292-307.
【3】国家卫生健康委员会,农业农村部,国家市场监督管理总局.食品安全国家标准食品中农药最大残留限量:GB 2763-2021[S].北京:中国标准出版社, 2021.
【4】CVJETKO BUBALO M, AC'G URKO N, TOMAŠEVI AC'G M, et al. Green extraction of grape skin phenolics by using deep eutectic solvents[J]. Food Chemistry, 2016,200:159-166.
【5】SMITH E L, ABBOTT A P, RYDER K S. Deep eutectic solvents and their applications[J]. Chemical Reviews, 2014,114(21):11060-11082.
【6】GANO ZAHARADDEEN S, MJALLI FAROUQ S, TALAL A W, et al. Solubility of thiophene and dibenzothiophene in anhydrous FeCl3-and ZnCl2-based deep eutectic solvents[J]. Industrial & Engineering Chemistry Research, 2014,53(16):6815-6823.
【7】LI C P, ZHANG J J, LI Z, et al. Extraction desulfurization of fuels with 'metal ions’ based deep eutectic solvents (MDESs)[J]. Green Chemistry, 2016,18(13):3789-3795.
【8】MOHD Z H F, CHONG F K, ABDUL M M I. Extractive deep desulfurization of diesel using choline chloride-glycerol eutectic-based ionic liquid as a green solvent[J]. Fuel, 2017,192:10-17.
【9】ALOMAR M, HAYYAN M, ALSAADI M, et al. Glycerol-based deep eutectic solvents: Physical properties[J]. Journal of Molecular Liquids, 2013,215:137-141.
【10】赵桐桐,张冬昊,郭振福,等.低共熔溶剂液相微萃取技术测定5种杀菌剂农药残留分析方法[J].现代食品科技, 2019,35(8):281-286.
【11】王素利,郭振福,庚丽丽.基于低共熔溶剂的液液微萃取技术测定食用油中的新烟碱类杀虫剂[J].食品科学, 2021,42(8):277-282.
【12】郭振福,庚丽丽,王素利.羟基离子液体磁性氧化石墨烯混合半胶束磁性固相萃取高效液相色谱测定环境水中的除草剂[J].环境化学, 2021,40(8):2561-2568.
【13】HEO J, YOON Y, LEE G, et al. Enhanced adsorption of bisphenol A and sulfamethoxazole by a novel magnetic CuZnFe2O4-biochar composite[J]. Bioresource Technology, 2019,281:179-187.
【14】NEJATI K, ZABIHI R. Preparation and magnetic properties of nano size nickel ferrite particles using hydrothermal method[J]. Chemistry Central Journal, 2012,6:1-6.
【15】王雪,孟令友,代莹,等.Fe3O4@SiO2-NH2磁性复合材料对水中单宁酸的吸附性能研究[J].环境科学学报, 2013,33(8):2193-2198.
【16】黄艳花.基于绿色溶剂的磁性固相萃取技术在蛋白质分离中的应用研究[D].长沙:湖南大学, 2016.
【2】CHAWLA P, KAUSHIK R, SHIVA SWARAJ V J, et al. Organophosphorus pesticides residues in food and their colorimetric detection[J]. Environmental Nanotechnology, Monitoring & Management, 2018,10:292-307.
【3】国家卫生健康委员会,农业农村部,国家市场监督管理总局.食品安全国家标准食品中农药最大残留限量:GB 2763-2021[S].北京:中国标准出版社, 2021.
【4】CVJETKO BUBALO M, AC'G URKO N, TOMAŠEVI AC'G M, et al. Green extraction of grape skin phenolics by using deep eutectic solvents[J]. Food Chemistry, 2016,200:159-166.
【5】SMITH E L, ABBOTT A P, RYDER K S. Deep eutectic solvents and their applications[J]. Chemical Reviews, 2014,114(21):11060-11082.
【6】GANO ZAHARADDEEN S, MJALLI FAROUQ S, TALAL A W, et al. Solubility of thiophene and dibenzothiophene in anhydrous FeCl3-and ZnCl2-based deep eutectic solvents[J]. Industrial & Engineering Chemistry Research, 2014,53(16):6815-6823.
【7】LI C P, ZHANG J J, LI Z, et al. Extraction desulfurization of fuels with 'metal ions’ based deep eutectic solvents (MDESs)[J]. Green Chemistry, 2016,18(13):3789-3795.
【8】MOHD Z H F, CHONG F K, ABDUL M M I. Extractive deep desulfurization of diesel using choline chloride-glycerol eutectic-based ionic liquid as a green solvent[J]. Fuel, 2017,192:10-17.
【9】ALOMAR M, HAYYAN M, ALSAADI M, et al. Glycerol-based deep eutectic solvents: Physical properties[J]. Journal of Molecular Liquids, 2013,215:137-141.
【10】赵桐桐,张冬昊,郭振福,等.低共熔溶剂液相微萃取技术测定5种杀菌剂农药残留分析方法[J].现代食品科技, 2019,35(8):281-286.
【11】王素利,郭振福,庚丽丽.基于低共熔溶剂的液液微萃取技术测定食用油中的新烟碱类杀虫剂[J].食品科学, 2021,42(8):277-282.
【12】郭振福,庚丽丽,王素利.羟基离子液体磁性氧化石墨烯混合半胶束磁性固相萃取高效液相色谱测定环境水中的除草剂[J].环境化学, 2021,40(8):2561-2568.
【13】HEO J, YOON Y, LEE G, et al. Enhanced adsorption of bisphenol A and sulfamethoxazole by a novel magnetic CuZnFe2O4-biochar composite[J]. Bioresource Technology, 2019,281:179-187.
【14】NEJATI K, ZABIHI R. Preparation and magnetic properties of nano size nickel ferrite particles using hydrothermal method[J]. Chemistry Central Journal, 2012,6:1-6.
【15】王雪,孟令友,代莹,等.Fe3O4@SiO2-NH2磁性复合材料对水中单宁酸的吸附性能研究[J].环境科学学报, 2013,33(8):2193-2198.
【16】黄艳花.基于绿色溶剂的磁性固相萃取技术在蛋白质分离中的应用研究[D].长沙:湖南大学, 2016.
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