Development of Dispersive Liquid-Liquid Microextraction Procedure for Trace Determination of Malathion Pesticide in Urine Samples
-
Maryam RAMIN
,
Monireh KHADEM
,
Fariborz OMIDI
,
Mehran POURHOSEIN
,
Farideh GOLBABAEI
,
Seyed Jamaleddin SHAHTAHERI
Abstract
Background: Measurement of pesticides in biological matrices is become a serious challenge for researches because of their very low concentration in different matrices. The aim of this study was to develop a new sam-ple preparation method with high accuracy and validity, simplicity and short retention time for determination of malathion.
Methods: Dispersive liquid-liquid micro-extraction (DLLME) technique coupled with high-performance liq-uid chromatography equipped with ultraviolet detector (HPLC-UV) developed for trace extraction and deter-mination of malathion pesticide in human urine samples. This study was done in 2017 at Tehran University of Medical Sciences, Tehran, Iran. One variable at a time (OVAT) method was used to optimize parameters af-fecting the malathion extraction. Different parameters such as extraction solvent, disperser solvent, and vol-ume of the extraction solvent, volume of the disperser solvent, centrifugation time and speed, salt addition, and sample pH were studied and optimized.
Results: Under the optimized conditions, the limit of detection and enrichment factor of the method were 0.5 μg L-1 and 200, respectively. The calibration curve was linear in the concentration range of 2-250 μg L-1. The relative standard deviation for six replicate experiments at 200 μg L-1 concentration was less than 3%. The rela-tive recoveries of spiked urine samples were 96.3%, 101.7% and 97.3% at three different concentration levels of 50, 200 and 1000 μg L-1, respectively.
Conclusion: DLLME procedure was successfully developed for the extraction of malathion from human urine samples. Compared to other extraction techniques, the proposed procedure had some advantages such as shorter extraction time, better reproducibility, and higher enrichment factor.
1. Barata C, Solayan A, Porte C (2004). Role of B-esterases in assessing toxicity of or-ganophosphorus (chlorpyrifos, malathi-on) and carbamate (carbofuran) pesti-cides to Daphnia magna. Aquat Toxicol, 66 (2): 125–139.
2. Rezaee M, Assadi Y, Milani Hosseini MR et al (2006). Determination of organic com-pounds in water using dispersive liquid-liquid microextraction. J Chromatogr A, 1116 (1): 1-9.
3. Peng JF, Liu JF, Hu XL, Jiang GB (2007). Direct determination of chlorophenols in environmental water samples by hollow fiber supported ionic liquid membrane extraction coupled with high-performance liquid chromatography. J Chromatogr A, 1139 (2): 165–170.
4. Omidi F, Behbahani M, Bojdi MK, Shahtaheri SJ (2015). Solid phase extrac-tion and trace monitoring of cadmium ions in environmental water and food samples based on modified magnetic na-noporous silica. J Magn Magn Mater, 395 (1): 213-220.
5. Saraji M, Boroujeni MK (2014). Recent de-velopments in dispersive liquid–liquid mi-croextraction. Anal Bioanal Chem, 406 (8): 2027–2066.
6. Behbahani M, Najafi F, Bagheri S et al (2013). Application of surfactant assisted dispersive liquid–liquid microextraction as an efficient sample treatment technique for preconcentration and trace detection of zonisamide and carbamazepine in urine and plasma samples. J Chromatog A, 1308: 25-31.
7. Herrera-Herrera AV, Asensio-Ramos M, Hernandez-Borges J, Rodriguez-Delgado MA (2010). Dispersive liquid-liquid mi-croextraction for determination of organ-ic analytes. Trends Anal Chem, 29 (7): 728–751.
8. El-Shahawi M, Al-Saidi H (2013). Dispersive liquid-liquid microextraction for chemical speciation and determination of ultra-trace concentrations of metal ions. Trends Anal Chem, 44 (1): 12–24.
9. Behbahani M, Najafi F, Bagheri S et al (2014). Coupling of solvent-based de-emulsification dispersive liquid–liquid mi-croextraction with high performance liq-uid chromatography for simultaneous simple and rapid trace monitoring of 2, 4-dichlorophenoxyacetic acid and 2-methyl-4-chlorophenoxyacetic acid. Envi-ron Monit Assess, 186 (4): 2609-18.
10. Kocurova L, Balogh IS, Šandrejova J, An-druch V (2012). Recent advances in dis-persive liquid–liquid microextraction us-ing organic solvents lighter than water. Microchem J, 102 (1): 11–17.
11. Spietelun A, Marcinkowski L, Guardia M, Namies nik J (2014). Green aspects, de-velopments and perspectives of liquid phase microextraction techniques. Talanta, 119 (3): 34–45.
12. Leong MI, Fuh MR, Huang SD (2014). Be-yond dispersive liquid–liquid microextrac-tion. J Chromatogr A, 1335 (1): 2–14.
13. Vinas P, Campillo N, Lopez-Garcia I, Her-nandez-Cordoba M (2014). Dispersive liquid–liquid microextraction in food analysis. Anal Bioanal Chem, 406 (8): 2067–2099.
14. Ma J, Lu W, Chen L (2012). Recent advanc-es in dispersive liquid-liquid microextrac-tion for organic compounds analysis in environmental water. Curr Anal Chem, 8 (1): 78–90.
15. Hossien-poor-Zaryabi M, Chamsaz M, Hei-dari T et al (2014). Application of disper-sive liquid–liquid micro-extraction using mean centering of ratio spectra method for trace determination of mercury in food and environmental samples. Food Anal Method, 7 (2): 352-9.
16. Farajzadeh MA, Sorouraddin SM, Mogaddam MRA (2014). Liquid phase microextraction of pesticides: a review on current methods. Microchim Acta, 181 (9): 829–851.
17. Alves ACH, Goncalves MMPB, Bernardo MMS, Mendes BS (2011). Validated dis-persive liquid–liquid microextraction for analysis of organophosphorous pesti-cides in water. J Sep Sci, 34 (11): 1326–1332.
18. Cinelli G, Avino P, Notardonato I, Russo MV (2014). Ultrasound-vortex-assisted dispersive liquid–liquid microextraction coupled with gas chromatography with a nitrogen–phosphorus detector for simul-taneous and rapid determination of or-ganophosphorus pesticides and triazines in wine. Anal Methods, 6 (3): 782–790.
19. Pourhossein M, Shahtaheri SJ, Maleck Khani H et al (2017). Optimization of dispersive liquid liquid microextraction method for determination of trace sali-vary melatonin using high performance liquid chromatography. Iran Occup Heal J, 14 (4): 85-94.
20. Naeeni MH, Yamini Y, Rezaee M (2011). Combination of supercritical fluid extrac-tion with dispersive liquid–liquid microex-traction for extraction of organophos-phorus pesticides from soil and marine sediment samples. J Supercrit Fluids, 57 (3): 219–226.
21. Ho YM, Tsoi YK, Leung KSY (2013). High-ly sensitive and selective organophos-phate screening in twelve commodities of fruits, vegetables and herbal medicines by dispersive liquid–liquid microextraction. Anal Chim Acta, 775 (2): 58–66.
22. Sanagi MMM, Miskam SU, Ibrahim MA, Wan WA (2011). Determination of or-ganophosphorus pesticides by dispersive liquid-liquid micro extraction coupled with gas chromatography-electron cap-ture detection. Malays J Anal Sci, 15 (2): 232–239.
23. Sousa R, Homem V, Moreira JL, Madeira LM, Alves A (2013). Optimisation and application of dispersive liquid–liquid mi-croextraction for simultaneous determi-nation of carbamates and organophos-phorus pesticides in waters. Anal Methods, 5 (11): 2736–2745.
24. Asfaram A, Ghaedi M, Goudarzi A, Soylak M (2015). Comparison between disper-sive liquid-liquid microextraction and ul-trasound-assisted nanoparticles-dispersive solid-phase microextraction combined with microvolume spectro-photometry method for the determina-tion of Auramine-O in water samples. RSC Advance, 5 (49): 39084-39096.
25. Wu C, Liu H, Liu W et al (2010). Determina-tion of organophosphorus pesticides in environmental water samples by disper-sive liquid–liquid microextraction with so-lidification of floating organic droplet fol-lowed by high-performance liquid chro-matography. Anal Bioanal Chem, 397 (6): 2543–2549.
26. Amelin V, Lavrukhin D, Tret yakov A (2013). Dispersive liquid-liquid microex-traction for the determination of herbi-cides of urea derivatives family in natural waters by HPLC. J Anal Chem, 68 (9): 822–830.
27. Mukdasai S, Thomas C, Srijaranai S (2014). Two-step microextraction combined with high performance liquid chromatographic analysis of pyrethroids in water and vege-table samples. Talanta, 120 (1): 289–296.
28. Boonchiangma S, Ngeontae W, Srijaranai S (2012). Determination of six pyrethroid insecticides in fruit juice samples using dispersive liquid–liquid microextraction combined with high performance liquid chromatography. Talanta, 88 (1): 209–215.
29. Shan H (2013). Simultaneous determination of six neonicotinoid residues in soil using DLLME-HPLC and UV. Guang Pu Xue Yu Guang Pu Fen Xi, 33 (9): 2553–2557.
30. Yao ZW, Jiang GB, Liu JM, Cheng W (2001). Application of solid–phase mi-croextraction for the determination of organophosphorous pesticides in aque-ous samples by gas chromatography with flame photometric detector. Talanta, 55 (4): 807–814.
31. Wang Y, Wang Z, Zhang H et al (2011). Application of pneumatic nebulization single-drop microextraction for the de-termination of Organophosphorous pes-ticides by gas chromatography–mass spectrometry. J Sep Sci, 34 (15): 1880–1885.
32. Farajzadeh MA, Asghari A, Feriduni B (2016). An efficient, rapid and micro-wave-accelerated dispersive liquid–liquid microextraction method for extraction and pre-concentration of some organo-phosphorus pesticide residues from aqueous samples. J Food Compos Anal, 48 (1): 73–80.
33. Habila MA, Al Othman ZA, Al-Tamrah SA et al (2015). Activated carbon from waste as an efficient adsorbent for malathion for detection and removal purposes. J Ind Eng Chem, 32: 336-344.
2. Rezaee M, Assadi Y, Milani Hosseini MR et al (2006). Determination of organic com-pounds in water using dispersive liquid-liquid microextraction. J Chromatogr A, 1116 (1): 1-9.
3. Peng JF, Liu JF, Hu XL, Jiang GB (2007). Direct determination of chlorophenols in environmental water samples by hollow fiber supported ionic liquid membrane extraction coupled with high-performance liquid chromatography. J Chromatogr A, 1139 (2): 165–170.
4. Omidi F, Behbahani M, Bojdi MK, Shahtaheri SJ (2015). Solid phase extrac-tion and trace monitoring of cadmium ions in environmental water and food samples based on modified magnetic na-noporous silica. J Magn Magn Mater, 395 (1): 213-220.
5. Saraji M, Boroujeni MK (2014). Recent de-velopments in dispersive liquid–liquid mi-croextraction. Anal Bioanal Chem, 406 (8): 2027–2066.
6. Behbahani M, Najafi F, Bagheri S et al (2013). Application of surfactant assisted dispersive liquid–liquid microextraction as an efficient sample treatment technique for preconcentration and trace detection of zonisamide and carbamazepine in urine and plasma samples. J Chromatog A, 1308: 25-31.
7. Herrera-Herrera AV, Asensio-Ramos M, Hernandez-Borges J, Rodriguez-Delgado MA (2010). Dispersive liquid-liquid mi-croextraction for determination of organ-ic analytes. Trends Anal Chem, 29 (7): 728–751.
8. El-Shahawi M, Al-Saidi H (2013). Dispersive liquid-liquid microextraction for chemical speciation and determination of ultra-trace concentrations of metal ions. Trends Anal Chem, 44 (1): 12–24.
9. Behbahani M, Najafi F, Bagheri S et al (2014). Coupling of solvent-based de-emulsification dispersive liquid–liquid mi-croextraction with high performance liq-uid chromatography for simultaneous simple and rapid trace monitoring of 2, 4-dichlorophenoxyacetic acid and 2-methyl-4-chlorophenoxyacetic acid. Envi-ron Monit Assess, 186 (4): 2609-18.
10. Kocurova L, Balogh IS, Šandrejova J, An-druch V (2012). Recent advances in dis-persive liquid–liquid microextraction us-ing organic solvents lighter than water. Microchem J, 102 (1): 11–17.
11. Spietelun A, Marcinkowski L, Guardia M, Namies nik J (2014). Green aspects, de-velopments and perspectives of liquid phase microextraction techniques. Talanta, 119 (3): 34–45.
12. Leong MI, Fuh MR, Huang SD (2014). Be-yond dispersive liquid–liquid microextrac-tion. J Chromatogr A, 1335 (1): 2–14.
13. Vinas P, Campillo N, Lopez-Garcia I, Her-nandez-Cordoba M (2014). Dispersive liquid–liquid microextraction in food analysis. Anal Bioanal Chem, 406 (8): 2067–2099.
14. Ma J, Lu W, Chen L (2012). Recent advanc-es in dispersive liquid-liquid microextrac-tion for organic compounds analysis in environmental water. Curr Anal Chem, 8 (1): 78–90.
15. Hossien-poor-Zaryabi M, Chamsaz M, Hei-dari T et al (2014). Application of disper-sive liquid–liquid micro-extraction using mean centering of ratio spectra method for trace determination of mercury in food and environmental samples. Food Anal Method, 7 (2): 352-9.
16. Farajzadeh MA, Sorouraddin SM, Mogaddam MRA (2014). Liquid phase microextraction of pesticides: a review on current methods. Microchim Acta, 181 (9): 829–851.
17. Alves ACH, Goncalves MMPB, Bernardo MMS, Mendes BS (2011). Validated dis-persive liquid–liquid microextraction for analysis of organophosphorous pesti-cides in water. J Sep Sci, 34 (11): 1326–1332.
18. Cinelli G, Avino P, Notardonato I, Russo MV (2014). Ultrasound-vortex-assisted dispersive liquid–liquid microextraction coupled with gas chromatography with a nitrogen–phosphorus detector for simul-taneous and rapid determination of or-ganophosphorus pesticides and triazines in wine. Anal Methods, 6 (3): 782–790.
19. Pourhossein M, Shahtaheri SJ, Maleck Khani H et al (2017). Optimization of dispersive liquid liquid microextraction method for determination of trace sali-vary melatonin using high performance liquid chromatography. Iran Occup Heal J, 14 (4): 85-94.
20. Naeeni MH, Yamini Y, Rezaee M (2011). Combination of supercritical fluid extrac-tion with dispersive liquid–liquid microex-traction for extraction of organophos-phorus pesticides from soil and marine sediment samples. J Supercrit Fluids, 57 (3): 219–226.
21. Ho YM, Tsoi YK, Leung KSY (2013). High-ly sensitive and selective organophos-phate screening in twelve commodities of fruits, vegetables and herbal medicines by dispersive liquid–liquid microextraction. Anal Chim Acta, 775 (2): 58–66.
22. Sanagi MMM, Miskam SU, Ibrahim MA, Wan WA (2011). Determination of or-ganophosphorus pesticides by dispersive liquid-liquid micro extraction coupled with gas chromatography-electron cap-ture detection. Malays J Anal Sci, 15 (2): 232–239.
23. Sousa R, Homem V, Moreira JL, Madeira LM, Alves A (2013). Optimisation and application of dispersive liquid–liquid mi-croextraction for simultaneous determi-nation of carbamates and organophos-phorus pesticides in waters. Anal Methods, 5 (11): 2736–2745.
24. Asfaram A, Ghaedi M, Goudarzi A, Soylak M (2015). Comparison between disper-sive liquid-liquid microextraction and ul-trasound-assisted nanoparticles-dispersive solid-phase microextraction combined with microvolume spectro-photometry method for the determina-tion of Auramine-O in water samples. RSC Advance, 5 (49): 39084-39096.
25. Wu C, Liu H, Liu W et al (2010). Determina-tion of organophosphorus pesticides in environmental water samples by disper-sive liquid–liquid microextraction with so-lidification of floating organic droplet fol-lowed by high-performance liquid chro-matography. Anal Bioanal Chem, 397 (6): 2543–2549.
26. Amelin V, Lavrukhin D, Tret yakov A (2013). Dispersive liquid-liquid microex-traction for the determination of herbi-cides of urea derivatives family in natural waters by HPLC. J Anal Chem, 68 (9): 822–830.
27. Mukdasai S, Thomas C, Srijaranai S (2014). Two-step microextraction combined with high performance liquid chromatographic analysis of pyrethroids in water and vege-table samples. Talanta, 120 (1): 289–296.
28. Boonchiangma S, Ngeontae W, Srijaranai S (2012). Determination of six pyrethroid insecticides in fruit juice samples using dispersive liquid–liquid microextraction combined with high performance liquid chromatography. Talanta, 88 (1): 209–215.
29. Shan H (2013). Simultaneous determination of six neonicotinoid residues in soil using DLLME-HPLC and UV. Guang Pu Xue Yu Guang Pu Fen Xi, 33 (9): 2553–2557.
30. Yao ZW, Jiang GB, Liu JM, Cheng W (2001). Application of solid–phase mi-croextraction for the determination of organophosphorous pesticides in aque-ous samples by gas chromatography with flame photometric detector. Talanta, 55 (4): 807–814.
31. Wang Y, Wang Z, Zhang H et al (2011). Application of pneumatic nebulization single-drop microextraction for the de-termination of Organophosphorous pes-ticides by gas chromatography–mass spectrometry. J Sep Sci, 34 (15): 1880–1885.
32. Farajzadeh MA, Asghari A, Feriduni B (2016). An efficient, rapid and micro-wave-accelerated dispersive liquid–liquid microextraction method for extraction and pre-concentration of some organo-phosphorus pesticide residues from aqueous samples. J Food Compos Anal, 48 (1): 73–80.
33. Habila MA, Al Othman ZA, Al-Tamrah SA et al (2015). Activated carbon from waste as an efficient adsorbent for malathion for detection and removal purposes. J Ind Eng Chem, 32: 336-344.
| Files | ||
| Issue | Vol 48 No 10 (2019) | |
| Section | Original Article(s) | |
| DOI | https://doi.org/10.18502/ijph.v48i10.3498 | |
| Keywords | ||
| Malathion Dispersive liquid-liquid microextraction One variable at a time Urine HPLC | ||
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How to Cite
1.
RAMIN M, KHADEM M, OMIDI F, POURHOSEIN M, GOLBABAEI F, SHAHTAHERI SJ. Development of Dispersive Liquid-Liquid Microextraction Procedure for Trace Determination of Malathion Pesticide in Urine Samples. Iran J Public Health. 2019;48(10):1893-1902.
