Abstract
Study conducted to develop and validate laboratory method using QuEChERS method. QuEChER method was used for the determination of 28 pesticide residues belongs to organochlorine, synthetic pyrethroids and herbicides in Spinach. Sample was extracted by ethyl acetate. Removal of moisture using from sample extract by anhydrous sodium sulphate and magnesium sulphate. Cleaning of matrix and other interferences was done by Primary Secondary Amine (PSA), C18 and activated charcoal. Agilent 7890B model GC-ECD with 7693 auto sampler and 7890A-Agilent Technologies GC with 5975C inert XL EI/CI MSD triple axis mass detector with DB-5MS fused silica capillary column were used for analysis of samples taken for study. Each pesticide spiking concentration was 0.05 ppm level in three replicate whose recovery lies between Codex permissible limit i.e. 70–120%. Relative standard deviation (RSD) < 15%. Codex norms were followed for repeatability and reproducibility check of the instrument. For Linearity check, taking area of lambda cyhalothrin against five different concentration levels of 0.003, 0.010, 0.100, 0.70, 1.00 mg/kg, calibration curve was plotted with regression co-efficient (r2) 0.993. Total uncertainty or combined uncertainty comprise of three main independent uncertainties arise due to weighing of standards, purity of the standard and repeatability of instruments. Expanded uncertainty is twice of the combined uncertainty which lies in three ranges viz., (a) ≤10% (b) 11–15% and (c) 15–20%. All pesticides taken for study were in the range (a) i.e. ≤10%.
This is a preview of subscription content, log in via an institution to check access.
Access this chapter
Tax calculation will be finalised at checkout
Purchases are for personal use only
References
Anastassiades M, Lehotay SJ, Stajnbaher 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 86:412–431
Hernandez-Borges J, Cabrera JC, Rodriguez-Delgado MA et al (2009) Analysis of pesticide residues in bananas harvested in the Canary Islands (Spain). Food Chem 113:313–319
Lehotay SJ, De Kok A, Hiemstra M et al (2005) Validation of a fast and easy method for the determination of residues from 229 pesticides in fruits and vegetables using gas and liquid chromatography and mass spectrometric detection. J AOAC Int 88:595–614
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
Paya P, Anastassiades M, Mack D et al (2007) Analysis of pesticide residues using the Quick Easy Cheap Effective Rugged and Safe (QuEChERS) pesticide multiresidue method in combination with gas and liquid chromatography and tandem mass spectrometric detection. Anal Bioanal Chem 389:1697–1714
Lehotay SJ (2007) Determination of pesticide residues in foods by acetonitrile extraction and partitioning with magnesium sulfate: collaborative study. J AOAC Int 90:485–520
EURACHEM/CITAC Guide CG 4, EURACHEM/ CITAC Guide (2000) Quantifying uncertainty in analytical measurement, 2nd ed
Sanyal D, Rani A, Alam S et al (2011) Development validation and uncertainty measurement of multi-residue analysis of organochlorine and organophosphorus pesticides using pressurized liquid extraction and dispersive-SPE techniques. Environ Monit Assess 182:97–113
Saini MK, Mishra S, Alam S et al (2016) Method development and validation of multiclass pesticide residues and metabolites in wheat by GC-ECD and GC-MS. Asian J Res Chem 9(1):1–9
Mishra S, Saini MK, Alam S et al (2015) Determination of 25 pesticides By GC-ECD And MSD with measurement of uncertainty in tomato using modified QuEChERS technique. J Appl Chem 4(1):221–231
Corley J (2002) Best practices in establishing detection and quantification limits for pesticide residues in foods. Rutgers, The State University of New Jersey, North Brunswick, NJ, USA
Corley J (2003) Best practices in establishing detection and quantification limits for pesticide residues in foods. In: Handbook of residue analytical methods for agrochemicals. Wiley, New York, USA, pp 59–74
Corley J (2005) Handbook of residue analytical methods for agrochemicals. Wiley, p. 59
Acknowledgements
The authors are highly grateful to the Director, Institute of Pesticide Formulation Technology for allowing them to use the research facilities for the work.
Conflict of Interest
The authors declare no conflict of interest.
Author information
Authors and Affiliations
Corresponding author
Editor information
Editors and Affiliations
Rights and permissions
Copyright information
© 2018 Springer Nature Singapore Pte Ltd.
About this paper
Cite this paper
Mishra, S., Richhariya, N., Alam, S., Thakur, L.K. (2018). In House Laboratory Method Validation and Uncertainty Determination of 28 Pesticides in Spinach by Gas Chromatography Using Electron Capture (ECD) and Mass Spectrometric (MS) Detector. In: Parmar, V., Malhotra, P., Mathur, D. (eds) Green Chemistry in Environmental Sustainability and Chemical Education. Springer, Singapore. https://doi.org/10.1007/978-981-10-8390-7_17
Download citation
DOI: https://doi.org/10.1007/978-981-10-8390-7_17
Published:
Publisher Name: Springer, Singapore
Print ISBN: 978-981-10-8389-1
Online ISBN: 978-981-10-8390-7
eBook Packages: Chemistry and Materials ScienceChemistry and Material Science (R0)