Fast Preconcentration of Pesticide Residues in Oilseeds by Combination of QuEChERS with Dispersive Liquid–Liquid Microextraction Followed by Gas Chromatography-Mass Spectrometry
- 357 Downloads
A fast, efficient, and simple method for determination of pesticide residues in pumpkin seeds has been developed combining QuEChERS and dispersive liquid–liquid microextraction (DLLME) followed by gas chromatography and mass spectrometry (GC-MS). Parameters affecting the DLLME performance such as solvent selection and volume of extractive and dispersive solvent, salt effect, and extraction time were studied. Under the selected conditions (50 μL extractive solvent chloroform, 1 mL QuEChERS extract, and 3 mL water), the developed method was validated. Linearity was evaluated at nine concentrations in the broad range of 0.1–500 μg/kg with correlation coefficients from 0.9842 to 0.9972. The relative standard deviations at lowest calibration level varied from 0.3 to 22 %. Under the optimum conditions, an enrichment factor was 6–17-fold and detection limits 0.01–12.17 μg/kg were achieved. Finally, the developed and validated method was successfully applied for the extraction and determination of pesticide residues in 16 real samples with 2 positive findings below maximum residue limits (MRL). Limits of detection (LODs) of the proposed method are below the MRLs established by the European Union.
KeywordsDispersive liquid–liquid microextraction QuEChERS Oilseeds Validation
Compliance with Ethical Standards
This work was supported by the Scientific Grant Agency of the Ministry of Education of the Slovak Republic and the Academy of Sciences (VEGA, project no. 1/0503/14) and by the Slovak Research and Development Agency under contract no. APVV-0797-11.
Conflict of Interest
Mária Andraščíková declares that she has no conflict of interests. Svetlana Hrouzková declares that she has no conflict of interests.
This article does not contain any studies with human participants or animals performed by any of the authors.
- Anastassiades M, Lehotay SJ, Štajnbaher D, Schenck FJ (2003) Fast and easy multiresidue method employing acetonitrile extraction/partitioning and “dispersive solid-phase extraction” for the determination of pesticide residues in produce. J AOAC Int 86(2):412–431Google Scholar
- Deme P, Azmeera T, Devi BLAP, Jonnalagadda PR, Prasad RBN, Sarathi UVRV (2014) An improved dispersive solid-phase extraction clean-up method for the gas chromatography-negative chemical ionisation tandem mass spectrometric determination of multiclass pesticide residues in edible oils. Food Chem 142:144–151CrossRefGoogle Scholar
- EU pesticide database (2005) Regulation (EC) No 396/2005 of the European Parliament and of the Council of 23 February 2005 on maximum residue levels of pesticides in or on food and feed of plant and animal origin and amending Council Directive 91/414/EEC. Off J Eur Union L 70:1–16. [cited 2012 June 15]. Available from: http://ec.europa.eu/sanco_pesticides/public/index.cfm
- Farajzadeh MA, Vardast MBMR, Bamorowat M (2011) Dispersive liquid-liquid microextraction for the analysis of three organophosphorus pesticides in real samples by high performance liquid chromatography-ultraviolet detection and its optimization by experimental design. Microchim Acta 172:465–470CrossRefGoogle Scholar
- Lacina O, Zachariasova M, Urbanova J, Vaclavikova M, Cajka T, Hajslova J (2012) Critical assessment of extraction methods for the simultaneous determination of pesticide residues and mycotoxins in fruits, cereals, spices and oil seeds employing ultra-high performance liquid chromatography–tandem mass spectrometry. J Chromatogr A 1262:8–18CrossRefGoogle Scholar
- Lozowicka B, Jankowska M, Rutkowska E (2009) Comparison of two preparation procedures for determination of pesticides residues in oilseed rape by gas chromatography. Chem Anal 54(3):367–387Google Scholar
- Matsadiq G, Hu H-L, Ren H-B, Zhou Y-W, Lu L, Cheng J (2011) Quantification of multi-residue levels in peach juices, pulps and peels using dispersive liquid–liquid microextraction based on floating organic droplet coupled with gas chromatography-electron capture detection. J Chromatogr B 879:2113–2118CrossRefGoogle Scholar
- Melo A, Cunha SC, Mansilha C, Aguiar A, Pinho O, Ferreira IMPLVO (2012) Monitoring pesticide residues in greenhouse tomato by combining acetonitrile-based extraction with dispersive liquid–liquid microextraction followed by gas-chromatography–mass spectrometry. Food Chem 135:1071–1077CrossRefGoogle Scholar
- Ozkan A (2015) Determination of pesticide residues in some oilseeds and nuts using LC-MS/MS analysis. Fresenius Environ Bull 24(2a):615–620Google Scholar
- SANCO document (2013) Guidance document on analytical quality control and validation procedures for pesticide residues analysis in food and feed. Document No. SANCO/12571/2013 Available from: http://www.ec.europa.eufood/plant/pesticides/guidance_documents/docs/qualcontrol_en.pd
- Wang P, Yang X, Wang J, Cui J, Dong AJ, Zhao HT, Zhang LW, Wang ZY, Xu RB, Li WJ, Zhang YC, Zhang H, Jing J (2012) Multi-residue method for determination of seven neonicotinoid insecticides in grains using dispersive solid-phase extraction and dispersive liquid–liquid micro-extraction by high performance liquid chromatography. Food Chem 134:1691–1698CrossRefGoogle Scholar
- Xiong J, Hu B (2008) Comparison of hollow fiber liquid phase microextraction and dispersive liquid–liquid microextraction for the determination of organosulfur pesticides in environmental and beverage samples by gas chromatography with flame photometric detection. J Chromatogr A 1193:7–18CrossRefGoogle Scholar