Determination of Residues of 3 Methoxyacrylate Fungicides in Coarse Grains by High Performance Liquid Chromatography with Dispersive Liquid-Liquid Microextraction
摘 要
基于天然生物衍生溶剂的分散液液微萃取(DLLME),结合高效液相色谱法测定杂粮中嘧菌酯、吡唑醚菌酯、肟菌酯等3种甲氧基丙烯酸酯类杀菌剂的残留量。取过筛后的样品1.0 g于10 mL离心管中,加入800 μL乙腈(分散剂),涡旋,取上清液500 μL,加入200 μL 4-异丙基甲苯(天然生物衍生溶剂为萃取剂),混匀,然后迅速注入含有5 mL水和200 mg氯化钠的10 mL离心管中。离心8 min后,将离心管放入-18 ℃冷冻,取上层未被固化的萃取液进行分析。结果表明:3种甲氧基丙烯酸酯类杀菌剂的质量分数在0.5~100 mg·kg-1内与其对应的峰面积呈线性关系,检出限为0.17 mg·kg-1;对燕麦、大麦、黑麦、高粱、小米等阴性样品进行加标回收试验,3种甲氧基丙烯酸酯类杀菌剂的回收率为90.5%~107%,测定值的相对标准偏差(n=5)均小于6.0%。
Abstract
A method for the determination of residues of 3 methoxyacrylate fungicides, including azoxystrobin, pyraclostrobin and trifloxystrobin, in coarse grains by high performance liquid chromatography with dispersive liquid-liquid microextraction (DLLME) based on natural bioderived solvent was proposed. The sifted sample (1.0 g) was taken, and 800 μL of acetonitrile (as dispersant) was added for vortex. Then 500 μL of the supernatant was taken, and 200 μL of 4-isopropyl toluene (natural bioderived solvent as extractant) was added. After mixing well, the solution was quickly injected into a 10 mL-centrifuge tube containing 5 mL of water and 200 mg of sodium chloride. After centrifugation for 8 min, the centrifuge tube was frozen at -18 ℃, and the upper layer of unsolidified extract was taken for analysis. As shown by the results, linear relationships between values of mass fraction and peak area of 3 methoxyacrylate fungicides were kept in the range of 0.5-100 mg·kg-1, with detection limit of 0.17 mg·kg-1. Test for recovery was made on the negative samples of oat, barley, rye, sorghum and millet, giving results in the range of 90.5%-107%, and RSDs (n=5) of the determined values were less than 6.0%.
中图分类号 O657.72 DOI 10.11973/lhjy-hx202304011
所属栏目 工作简报
基金项目 山西省重点研发计划项目(202102140601018);山西省高等学校科技创新项目(2021L163)
收稿日期 2021/9/26
修改稿日期
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联系人作者王晓闻(wwxw11@163.com)
备注杨宏园,工程师,硕士,研究方向为食品检验检测
引用该论文: YANG Hongyuan,JING Xu,WANG Xiaowen. Determination of Residues of 3 Methoxyacrylate Fungicides in Coarse Grains by High Performance Liquid Chromatography with Dispersive Liquid-Liquid Microextraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2023, 59(4): 432~436
杨宏园,荆旭,王晓闻. 分散液液微萃取-高效液相色谱法测定杂粮中3种甲氧基丙烯酸酯类杀菌剂的残留量[J]. 理化检验-化学分册, 2023, 59(4): 432~436
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【7】孙悦,何莲芝,苏卓文,等.超声辅助低共熔溶剂提取甘草多糖的研究[J].食品研究与开发, 2021,42(2):84-91.
【8】张琰,赵其阳,张耀海,等.温控辅助离子液体分散液液微萃取-高效液相色谱检测果汁中杀菌剂残留[J].食品科学, 2015,36(4):202-207.
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【10】WANG C, WU Q H, WU C X, et al. Application of dispersion-solidification liquid-liquid microextraction for the determination of triazole fungicides in environmental water samples by high-performance liquid chromatography[J]. Journal of Hazardous Materials, 2011,185(1):71-76.
【11】王东,侯传金,赵尔成,等.分散液液微萃取/气相色谱-质谱法测定蜂蜜中六六六和滴滴涕类农药残留[J].色谱, 2015,33(1):40-45.
【12】李祖光,宋志宇,劳家正,等.新型分散液液微萃取-GC/MS检测水中三唑类农残[J].浙江工业大学学报, 2017,45(2):190-194.
【13】BESSAIRE T, MUJAHID C, BECK A, et al. Screening of 23 β-lactams in foodstuffs by LC-MS/MS using an alkaline QuEChERS-like extraction[J]. Food Additives&Contaminants:Part A, 2018,35(4):662-674.
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