Springer Nature is making Coronavirus research free. View research | View latest news | Sign up for updates

Determination of Organophosphorus Pesticides in Juice and Water by Modified Continuous Sample Drop Flow Microextraction Combined with Gas Chromatography–Mass Spectrometry


In this paper, the technique of continuous sample drop flow microextraction (CSDF-ME) is developed by the addition of a narrow-necked conical vessel. In the developed technique, an organic solvent denser than water is used for the extraction of organophosphorus pesticides (OPPs) from fruit juice and river water, followed by analysis with GC-MS. Eight milliliters of the sample solution is pumped at 0.5 mL min−1 flow rate into 12.0 μL extraction solvent (chloroform) and placed in the narrow-necked conical vessel for extraction and pre-concentration processes. Under optimal condition, the enrichment factor (EF) and linearity are found to be in the range of 102–380 and 500.0 μg L−1 with correlation coefficient greater than 0.98, respectively. The detection limit is in the range of 0.3–1.0 μg L−1 and LOQ ranged from 2.0–5.0 μg L−1. The relative standard division (RSD) of six replicate measurements for three different concentrations (i.e., 15.0, 50.0, 150.0 μg L−1) is 3.8–8.4%, 2.6–6.0%, and 2.2–4.8%, respectively. Values of RSD% of the target pesticides at 50.0 μg L−1 concentration levels are less than 6.0%.

This is a preview of subscription content, log in to check access.

Fig. 1
Fig. 2
Fig. 3
Fig. 4
Fig. 5
Fig. 6


  1. Ahmadi F, Assadi Y, Hosseini SMRM, Rezaee M (2006) Determination of organophosphorus pesticides in water samples by single drop microextraction and gas chromatography–flame photometric detector. J Chromatogr A 1101:307–312

  2. Ahmadi-Jouibari T, Pasdar Y, Pirsaheb M, Fattahi N (2017) Continuous sample drop flow-microextraction followed by high performance liquid chromatography for determination of triazine herbicides from fruit juices. Anal Method 9:980–985

  3. Alizadeh R, Kashkoei PK, Kazemipour M (2016) Zinc oxide-copper oxide nanoplates composite as coating for solid phase microextraction combined with high performance liquid chromatography-UV detection for trace analysis of chlorophenols in water and tomato juice samples. Anal Bioanal Chem 408:3727–3736

  4. ALOthman Z, Yilmaz E, Habila M, Abdelghfar A, Alhanaki B, Soylak M, Yacine A (2019) Supramolecular solvent microextraction and ultra-performance liquid chromatography-tandem mass spectrometry combination for the preconcentration and determination of malathion in environmental samples. Desalin Water Treat 144:166–171

  5. Andreu V, Picó Y (2012) Determination of currently used pesticides in biota. Anal Bioanal Chem 404:2659–2681

  6. Bayrami M, Hashemi T, Malekirad A, Ashayeri H, Faraji F, Abdollahi M (2012) Electroencephalogram, cognitive state, psychological disorders, clinical symptom, and oxidative stress in horticulture farmers exposed to organophosphate pesticides. Toxicol Ind Health 28:90–96

  7. Cacho JI, Campillo N, Vinas P, Hernandez-Cordoba M (2018) In situ ionic liquid dispersive liquid-liquid microextraction coupled to gas chromatography-mass spectrometry for the determination of organophosphorus pesticides. J Chromatogr A 1559:95–101

  8. Campillo N, Penalver R, Aguinaga N, Hernandez-Cordoba M (2006) Solid-phase microextraction and gas chromatography with atomic emission detection for multiresidue determination of pesticides in honey. Anal Chim Acta 562:9–15

  9. Chai MK, Tan GH (2009) Validation of a headspace solid-phase microextraction procedure with gas chromatography–electron capture detection of pesticide residues in fruits and vegetables. Food Chem 117:561–567

  10. Cooper J, Dobson H (2007) The benefits of pesticides to mankind and the environment. Crop Prot 26:1337–1348

  11. Farajzadeh MA, Sadeghi Alavian A, Sattari Dabbagh M (2019a) Development of an efficient sample preparation method based on homogeneous liquid-liquid extraction combined with dispersive liquid-liquid microextraction solidification of floating organic drop for trace analysis of pesticide residues in fruit and fruit juice samples. Food Anal Methods 12:2730–2741. https://doi.org/10.1007/s12161-019-01628-y

  12. Farajzadeh MA, Safi R, Yadeghari A (2019b) Combination of QuEChERS extraction with magnetic solid phase extraction followed by dispersive liquid–liquid microextraction as an efficient procedure for the extraction of pesticides from vegetable, fruit, and nectar samples having high content of solids. Microchem J 147:571–581

  13. Fernandes VC, Freitas M, Pacheco JG, Oliveira JM, Domingues VF, Delerue-Matos C (2018) Magnetic dispersive micro solid-phase extraction and gas chromatography determination of organophosphorus pesticides in strawberries. J Chromatogr A 1566:1–12

  14. Garcia AM (2003) Pesticide exposure and women’s health. Am J Ind Med 44:584–594

  15. He Y, Lee HK (2006) Continuous flow microextraction combined with high-performance liquid chromatography for the analysis of pesticides in natural waters. J Chromatogr A 1122:7–12

  16. Jouyban A, Farajzadeh MA, AfsharMogaddam MR (2018) A lighter-than-water deep eutectic-solvent-based dispersive liquid-phase microextraction method in a U-shaped homemade device. New J Chem 42:10100–10110

  17. Jouyban A, Farajzadeh MA, Afshar Mogaddam MR (2019) Dispersive liquid–liquid microextraction based on solidification of deep eutectic solvent droplets for analysis of pesticides in farmer urine and plasma by gas chromatography–mass spectrometry. J Chromatogr B 1124:114–121

  18. Karalliedde L (1999) Organophosphorus poisoning and anaesthesia. Anaesthesia 54:1073–1088

  19. Kharbouche L, Gil Garcia MD, Lozano A, Hamaizi H, Martinez Galera M (2019) Solid phase extraction of pesticides from environmental waters using an MSU-1 mesoporous material and determination by UPLC-MS/MS. Talanta 199:612–619

  20. McCauley LA, Anger WK, Keifer M, Langley R, Robson MG, Rohlman D (2006) Studying health outcomes in farmworker populations exposed to pesticides. Environ Health Perspect 114:953–960

  21. Moinfar S, Hosseini MRM (2009) Development of dispersive liquid–liquid microextraction method for the analysis of organophosphorus pesticides in tea. J Hazard Mater 169:907–911

  22. Moinfar S, Khayatian G (2017) Continuous sample drop flow-based microextraction combined with graphite furnace atomic absorption spectrometry for determination of cadmium. Microchem J 132:293–298

  23. Moinfar S, Khayatian G, Milani-Hosseini MR (2014) Continuous sample drop flow-based microextraction method as a microextraction technique for determination of organic compounds in water sample. Talanta 129:309–314

  24. Moinfar S, Khayatian G, Jamil LA (2018) Semi-automated continuous sample drop flow microextraction with swift preconcentration and atomic absorption spectrometry determination of lead in water and apple leaves. J Iran Chem Soc 15:2511–2518

  25. Moses M (1989) Pesticide-related health problems and farmworkers. AAOHN J 37:115–130

  26. Nguyen TD, Yu JE, Lee DM, Lee GH (2008) A multiresidue method for the determination of 107 pesticides in cabbage and radish using QuEChERS sample preparation method and gas chromatography mass spectrometry. Food Chem 110:207–213

  27. Rezaee M, Assadi Y, Hosseini MRM, Aghaee E, Ahmadi F, Berijani S (2006) Determination of organic compounds in water using dispersive liquid–liquid microextraction. J Chromatogr A 1116:1–9

  28. Sapahin HA, Makahleh A, Saad B (2014) Determination of organophosphorus pesticide residues in vegetables using solid phase micro-extraction coupled with gas chromatography–flame photometric detector. Arab J Chem in press. https://doi.org/10.1016/j.arabjc.2014.12.001

  29. Shamsipur M, Yazdanfar N, Ghambarian M (2016) Combination of solid-phase extraction with dispersive liquid-liquid microextraction followed by GC-MS for determination of pesticide residues from water, milk, honey and fruit juice. Food Chem 204:289–297

  30. Sun X, Zhu F, Xi J, Lu T, Liu H, Tong Y, Ouyang G (2011) Hollow fiber liquid-phase microextraction as clean-up step for the determination of organophosphorus pesticides residues in fish tissue by gas chromatography coupled with mass spectrometry. Mar Pollut Bull 63:102–107

  31. Van Der Werf HM (1996) Assessing the impact of pesticides on the environment. Agric Ecosyst Environ 60:81–96

  32. Wang YL, Zeng ZR, Liu MM, Yang M, Dong CZ (2008) Determination of organophosphorus pesticides in pakchoi samples by headspace solid-phase microextraction coupled with gas chromatography using home-made fiber. Eur Food Res Technol 226:1091–1098

  33. Wilson C, Tisdell C (2001) Why farmers continue to use pesticides despite environmental, health and sustainability costs. Ecol Econ 39:449–462

  34. Yang X, Zhang H, Liu Y, Wang J, Zhang YC, Dong AJ, Zhao HT, Sun CH, Cui J (2011) Multiresidue method for determination of 88 pesticides in berry fruits using solid-phase extraction and gas chromatography–mass spectrometry: determination of 88 pesticides in berries using SPE and GC–MS. Food Chem 127:855–865

  35. Yao ZW, Jiang GB, Liu JM, Cheng W (2001) Application of solid-phase microextraction for the determination of organophosphorus pesticides in aqueous samples by gas chromatography with flame photometric detector. Talanta 55:807–814

  36. Zacharis CK, Rotsias I, Zachariadis PG, Zotos A (2012) Dispersive liquid–liquid microextraction for the determination of organochlorine pesticides residues in honey by gas chromatography-electron capture and ion trap mass spectrometric detection. Food Chem 134:1665–1672

  37. Zhang R, Li N, Sun J, Gao F (2015) Colorimetric and phosphorimetric dual-signaling strategy mediated by inner filter effect for highly sensitive assay of organophosphorus pesticides. J Agric Food Chem 63:8947–8954

Download references


This work received financial support from the University of Zakho (Grant number SRS-0190118).

Author information

Correspondence to Soleyman Moinfar.

Ethics declarations

Conflict of Interest

Soleyman Moinfar declares that she has no conflict of interest. Lazgin Abdi Jamil declares that she has no conflict of interest. Helan Zeyad Sami declares that she has no conflict of interest.

Ethical Approval

This article does not contain any studies with human and animal subjects.

Informed Consent

Not applicable.

Additional information

Publisher’s Note

Springer Nature remains neutral with regard to jurisdictional claims in published maps and institutional affiliations.

Rights and permissions

Reprints and Permissions

About this article

Verify currency and authenticity via CrossMark

Cite this article

Moinfar, S., Jamil, L.A. & Sami, H.Z. Determination of Organophosphorus Pesticides in Juice and Water by Modified Continuous Sample Drop Flow Microextraction Combined with Gas Chromatography–Mass Spectrometry. Food Anal. Methods (2020). https://doi.org/10.1007/s12161-020-01723-5

Download citation


  • Organophosphorus pesticides
  • Continuous sample drop flow microextraction
  • Water
  • Juice
  • Gas chromatography–mass spectrometry