Food and Fermentation Industries >

2023 , Vol. 49 >Issue 20: 294 - 299

DOI: https://doi.org/10.13995/j.cnki.11-1802/ts.033212

Study on determination of 11 organophosphorus pesticide residues in vegetable oil samples by gas chromatography combined with dispersive liquid-liquid microextraction

  • LI Fangfang ,
  • WANG Yanli ,
  • LI Jie ,
  • CHEN Qianqian ,
  • TIAN Qiyan ,
  • CHEN Keyun ,
  • JU Xiang ,
  • ZHAO Fa ,
  • ZHANG Hui ,
  • LIU Yanming
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  • (Shandong Institute for Food and Drug Control, Key Laboratory of Supervising Technology for Meat and Meat Products for State Market Regulation, Shandong Research Center of Engineering and Technology for Quality Control of Food for Special Medical Purposes, Shandong Research Center of Engineering and Technology for Safety Inspection of Food and Drug, Jinan 250101, China)

Received date: 2022-08-05

  Revised date: 2022-11-04

  Online published: 2023-11-20

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Abstract

Based on green chemistry, a new method for the determination of 11 organophosphorus pesticide residues in vegetable oil was established, which selected green dispersive liquid-liquid microextraction as pre-treatment technology and gas chromatography-flame photometric detector with specificity for the detection of organophosphorus pesticides. The sample was dissolved in n-hexane, and extracted with N, N-dimethylformamide. The extraction solution was added with trace dichloromethane for dispersive liquid-liquid microextraction. The dichloromethane phase was detected by a flame photometric detector and quantified by an external standard method. The factors affecting the extraction efficiency were investigated, such as the conditions of sample extraction, the type and volume of extraction and dispersive solvent, and the concentration of sodium chloride. The best operational conditions were selected. Under the best operational conditions, the calibration curves were linear in the range of 0.01-1.00 μg/mL and the correlation coefficients were 0.999 1-0.999 7 for the 11 organophosphorus pesticides. The recoveries of the 11 organophosphorus pesticides ranged from 75.6% to 116.2% with relative standard deviation (RSD) values from 1.6% to 8.7% at three spiked levels of 0.01, 0.10, and 0.50 mg/kg. The limits of detection (LODs) were 0.002-0.003 mg/kg and the limits of quantification (LOQs) were 0.007-0.010 mg/kg. The method has been proven to be rapid, simple, and environmental-friendly, which is applicable to the determination of organophosphorus pesticides in vegetable oil.

Key words： dispersive liquid-liquid microextraction; gas chromatography; flame photometric detector; organophosphorus pesticide residues; vegetable oil

Cite this article

LI Fangfang , WANG Yanli , LI Jie , CHEN Qianqian , TIAN Qiyan , CHEN Keyun , JU Xiang , ZHAO Fa , ZHANG Hui , LIU Yanming . Study on determination of 11 organophosphorus pesticide residues in vegetable oil samples by gas chromatography combined with dispersive liquid-liquid microextraction[J]. Food and Fermentation Industries, 2023 , 49(20) : 294 -299 . DOI: 10.13995/j.cnki.11-1802/ts.033212

References

[1] 颜鸿飞, 张帆, 陈练, 等.在线凝胶渗透色谱-三重四极杆气质联用法同时测定橄榄油中72种农药残留[J].食品安全质量检测学报, 2016, 7(1):166-176.
YAN H F, ZHANG F, CHEN L, et al.Determination of 72 pesticide residues in olive oil by online gel permeation chromatography gas chromatography-tandem mass spectrometry[J].Journal of Food Safety and Quality, 2016, 7(1):166-176.
[2] FANG Y, TIAN W, PEI F, et al.Simultaneous determination of pesticide residues and antioxidants in blended oil using a liquid-liquid extraction combined with dispersive solid phase extraction method[J].Food Chemistry, 2017, 229:347-353.
[3] 史晓梅, 陈士恒, 章晴, 等.分散固相萃取-气相色谱法快速测定食用植物油中66种农药残留[J].中国粮油学报, 2016, 31(7):132-137.
SHI X M, CHEN S H, ZHANG Q, et al.Rapid determination of 66 pesticides residues in edible vegetable oil by dispersive solid phase extraction method-gas chromatography[J].Journal of the Chinese Cereals and Oils Association, 2016, 31(7):132-137.
[4] MORENO-GONZÁLEZ D, ALCÁNTARA-DURÁN J, ADDONA S M, et al.Multi-residue pesticide analysis in virgin olive oil by nanoflow liquid chromatography high resolution mass spectrometry[J].Journal of Chromatography A, 2018, 1562:27-35.
[5] CUI Y, KE R H, GAO W, et al.Analysis of organochlorine pesticide residues in various vegetable oils collected in Chinese markets[J].Journal of Agricultural and Food Chemistry, 2020, 68(49):14594-14602.
[6] 徐芷怡, 陈梦婷, 侯锡爱, 等.QuEChERS-高效液相色谱-串联质谱法同时测定芝麻油中7种农药残留[J].分析化学, 2020, 48(7):928-936.
XU Z Y,CHEN M T,HOU X A,et al.Simultaneous determination of seven pesticide residues in sesame oil using QuEChERS-high performance liquid chromatography-tandem mass spectrometry[J].Chinese Journal of Analytical Chemistry, 2020, 48(7):928-936.
[7] REZAEE M, ASSADI Y, MILANI HOSSEINI M R, et al.Determination of organic compounds in water using dispersive liquid-liquid microextraction[J].Journal of Chromatography A, 2006, 1116(1-2):1-9.
[8] ORTEGA-ZAMORA C, JIMÉNEZ-SKRZYPEK G, GONZÁLEZ-SÁLAMO J, et al.Extraction of phthalic acid esters from soft drinks and infusions by dispersive liquid-liquid microextraction based on the solidification of the floating organic drop using a menthol-based natural deep eutectic solvent[J].Journal of Chromatography A, 2021, 1646:46132.
[9] ORTEGA-ZAMORA C, GONZÁLEZ-SÁLAMO J, HERNÁNDEZ-SÁNCHEZ C, et al.Menthol-based deep eutectic solvent dispersive liquid-liquid microextraction:A simple and quick approach for the analysis of phthalic acid esters from water and beverage samples[J].ACS Sustainable Chemistry& Engineering, 2020, 8(23):8783-8794.
[10] FARAJZADEH M A, FAZLI N, PEZHHANFAR S, et al.Combination of a dispersive solid phase extraction method based on octadecylamine modified magnetic nanoparticles with dispersive liquid-liquid microextraction for the extraction and preconcentration of pesticides[J].Analytical Methods: Advancing Methods and Applications, 2022, 14(24):2376-2388.
[11] MARDANI A, AFSHAR MOGADDAM M R, FARAJZADEH M A, et al.A three-phase solvent extraction system combined with deep eutectic solvent-based dispersive liquid-liquid microextraction for extraction of some organochlorine pesticides in cocoa samples prior to gas chromatography with electron capture detection[J].Journal of Separation Science, 2020, 43(18):3674-3682.
[12] ABDALLAH O I, AHMED N S.Development of a vortex-assisted dispersive liquid-liquid microextraction (VA-DLLME) and LC-MS/MS procedure for simultaneous determination of fipronil and its metabolite fipronil sulfone in tomato fruits[J].Food Analytical Methods.2019, 12(10):2314-2325.
[13] 曹小云, 陈树干, 曾楚莹, 等.QuEChERS-分散液液微萃取/气相色谱-串联质谱法高通量快速检测蔬果中152种农药残留[J].分析测试学报, 2019, 38(8):920-930.
CAO X Y, CHEN S G, ZENG C Y, et al.High-throughput rapid detection of multi-pesticide residues in vegetables and fruits by gas chromatography-tandem mass spectrometry combined with QuEChERS-dispersed liquid-liquid microextraction[J].Journal of Instrumental Analysis, 2019, 38(8):775-778.
[14] ERCAN M S F, AYYÍLDÍZ M F, YAZÍCÍ E, et al.Development and validation of dispersive liquid-liquid microextraction method for the determination of 15 polycyclic aromatic hydrocarbons in 200 Antarctica samples by gas chromatography mass spectrometry[J].Environmental Monitoring and Assessment, 2022, 194(5):1-12.
[15] CALDEIRÃO L, FERNANDES J O, GONZALEZ M H, et al.A novel dispersive liquid-liquid microextraction using a low density deep eutectic solvent-gas chromatography tandem mass spectrometry for the determination of polycyclic aromatic hydrocarbons in soft drinks[J].Journal of Chromatography A, 2021, 1 635:461736.
[16] DING M Z, LIU W X, PENG J, et al.Simultaneous determination of seven preservatives in food by dispersive liquid-liquid microextraction coupled with gas chromatography-mass spectrometry[J].Food Chemistry, 2018, 269:187-192.
[17] 王晓春, 梁丽, 周焕英.基于QuEChERS净化/气相色谱法测定蔬菜及水果中16种有机氯农药残留[J].分析测试学报, 2021, 40(3):401-405.
WANG X C,LIANG L,ZHOU H Y.Determination of 16 organochlorine pesticides residues in vegetables and fruits by gas chromatography with QuEChERS purification[J].Journal of Instrumental Analysis, 2021, 40(3):401-405.
[18] 杨志敏, 常巧英, 李坚, 等.羟基多壁碳纳米管分散固相萃取/气相色谱-串联质谱法测定党参中75种农药残留[J].分析测试学报, 2022, 41(6):827-834.
YANG Z M,CHANG Q Y,LI J,et al.Determination of 75 pesticide residues in Codonopsis radix by gas chromatography-tandem mass spectrometry with dispersive solid phase extraction based on hydroxylated multi-walled carbon nanotubes[J].Journal of Instrumental Analysis, 2022, 41(6):827-834.
[19] 许芮菡, 谢倩文, 李旭军, 等.基于多壁碳纳米管改进QuEChERS法结合气相色谱-串联质谱检测茶叶中10种拟除虫菊酯类农药残留[J].色谱, 2022, 40(5):469-476.
XU R H,XIE Q W,LI X J,et al.Modified QuEChERS method based on multi-walled carbon nanotubes coupled with gas chromatography-tandem mass spectrometry for the detection of 10 pyrethroid pesticide residues in tea[J].Chinese Journal of Chromatography, 2022, 40(5):469-476.
[20] HIDALGO-RUIZ J L, ROMERO-GONZÁLEZ R, MARTÍNEZ VIDAL J L, et al.Monitoring of polar pesticides and contaminants in edible oils and nuts by liquid chromatography-tandem mass spectrometry[J].Food Chemistry, 2021, 343:128495.
[21] 宋伟, 周典兵, 郭春丽, 等.磁性富勒烯分散固相萃取-液相色谱-串联质谱法测定菊花中农药残留[J].分析化学, 2021, 49(9):1587-1596.
SONG W,ZHOU D B,GUO C L,et al.Determination of multiresidue of pesticide in chrysanthemum by magnetic fullerene dispersive solid phase extraction with liquid chromatography-tandem mass spectrometry[J].Chinese Journal of Analytical Chemistry, 2021, 49(9):1587-1596.
[22] 张艳侠, 赵慧男, 孙珊珊, 等.通过式SPE-UPLC-MS/MS测定植物油中的9种酚类抗氧化剂[J].食品科学, 2021, 42(10):322-329.
ZHANG Y X,ZHAO H N,SUN S S,et al.Simultaneous determination of nine phenolic antioxidants in vegetable oil by pass-through solid phase extraction cleanup and ultra-high performance liquid chromatography-tandem mass spectrometry[J].Food Science, 2021, 42(10):322-329.
[23] CUSTODIO-MENDOZA J A, AJA-MACAYA J, VALENTE I M, et al.Determination of malondialdehyde, acrolein and four other products of lipid peroxidation in edible oils by gas-diffusion microextraction combined with dispersive liquid-liquid microextraction[J].Journal of Chromatography A, 2020, 1627:461397.
[24] KHALILIAN F, REZAEE M.Ultrasound-assisted extraction followed by solid-phase extraction followed by dispersive liquid-liquid microextraction for the sensitive determination of diazinon and chlorpyrifos in rice[J].Food Analytical Methods, 2017, 10(4):885-891.
[25] 夏英, 张澜, 赵尔成, 等.分散固相萃取/分散液液微萃取-气相色谱法测定甘蓝中的拟除虫菊酯类农药残留[J].分析测试学报, 2014, 33(2):192-196.
XIA Y,ZHANG L,ZHAO E C,et al.Determination of pyrethroid residue in cabbage by gas chromatography combined with dispersive solid-phase extraction and dispersive liquid-liquid extraction[J].Journal of Instrumental Analysis, 2014, 33(2):192-196.
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