Method development for determination of multi-mycotoxin in vegetable oil using QuEChERS technique and liquid chromatography tandem mass spectrometry

In recent years, vegetable oils were reported to be contaminated by mycotoxins. At the same time, demand for vegetable oils has been increasing due to its health benefit and also for its direct use or as ingredients in food. The objectives of this study were to develop and validate the QuEChERS (Qui...

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Main Author:	Kuppan, Sharmili
Format:	Thesis
Language:	English
Published:	2015
Subjects:	Mycotoxins - Synthesis Vegetable oils Liquid chromatography
Online Access:	http://psasir.upm.edu.my/id/eprint/65744/1/FSTM%202015%2032IR.pdf
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spelling	my-upm-ir.657442018-10-16T02:04:18Z Method development for determination of multi-mycotoxin in vegetable oil using QuEChERS technique and liquid chromatography tandem mass spectrometry 2015-12 Kuppan, Sharmili In recent years, vegetable oils were reported to be contaminated by mycotoxins. At the same time, demand for vegetable oils has been increasing due to its health benefit and also for its direct use or as ingredients in food. The objectives of this study were to develop and validate the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) extraction and clean-up procedures for mycotoxins in vegetable oil by liquid chromatography tandem mass spectrometry (LC-MS/MS) and to verify the established method in vegetable oils in Malaysian market. In this study, a new, fast, cost efficient, sensitive and accurate assay method was developed, optimized and validated for the determination of aflatoxins (AFB1, AFB2, AFG1 and AFG2), ochratoxin A (OTA), zearalenone (ZEA) and deoxynivalenol (DON) in vegetable oil by a modified QuEChERS approach, which was conventionally developed for pesticides analysis. A quick procedure of mycotoxins extraction and clean-up was achieved in two steps. Firstly, target analytes were extracted into the optimized solvent acetonitrile and followed by dispersive solid phase extraction (dSPE) clean up with the optimized sorbents to remove the co-extracts. Three types of d-SPE sorbents; C18, primary secondary amine (PSA) and graphitized carbon black (GCB) and four combination ratios of two selected d-SPEs were evaluated to achieve an optimum and acceptable result. The maximum co-extracts were removed when d-SPE C18 and GCB were used at ratio 3:1 with MgSO4 anhydrous followed by LC-MS/MS analysis, using an electro spray-ionization interface (ESI). Methanol as an organic phase and formic acid (0.1%) with 5 mM ammonium acetate as a polar phase, with total run of 16 minutes and flow rate 300 µLmin-1 were applied. The validation study indicated the seven mycotoxins could be detected in the concentration range of 0.01 ngg-1 to650.17ngg-1 with correlation coefficient > 0.98. The limit of quantitation (LOQ) ranges from 0.04 ngg-1 to 2000 ngg-1. The recoveries were in the range of 87.9% to 106.6%. The repeatability and reproducibility of the analysis were within the acceptable level (0.5 – 1.3) for precision using HORRAT ratio. Significant matrix effect was compensated using the matrix matched calibration curves. After validation, the method was successfully applied to 25 vegetable oil samples including corn oil, palm oil and sunflower oil. ZEA, AFG2, AFG1 and AFB1 were among the detected mycotoxins. A new fast, cost efficient, sensitive and accurate assay method was successfully developed, validated and applied for the determination of seven mycotoxins in vegetable oils. Mycotoxins - Synthesis Vegetable oils Liquid chromatography 2015-12 Thesis http://psasir.upm.edu.my/id/eprint/65744/ http://psasir.upm.edu.my/id/eprint/65744/1/FSTM%202015%2032IR.pdf text en public masters Universiti Putra Malaysia Mycotoxins - Synthesis Vegetable oils Liquid chromatography
institution	Universiti Putra Malaysia
collection	PSAS Institutional Repository
language	English
topic	Mycotoxins - Synthesis Vegetable oils Liquid chromatography
spellingShingle	Mycotoxins - Synthesis Vegetable oils Liquid chromatography Kuppan, Sharmili Method development for determination of multi-mycotoxin in vegetable oil using QuEChERS technique and liquid chromatography tandem mass spectrometry
description	In recent years, vegetable oils were reported to be contaminated by mycotoxins. At the same time, demand for vegetable oils has been increasing due to its health benefit and also for its direct use or as ingredients in food. The objectives of this study were to develop and validate the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) extraction and clean-up procedures for mycotoxins in vegetable oil by liquid chromatography tandem mass spectrometry (LC-MS/MS) and to verify the established method in vegetable oils in Malaysian market. In this study, a new, fast, cost efficient, sensitive and accurate assay method was developed, optimized and validated for the determination of aflatoxins (AFB1, AFB2, AFG1 and AFG2), ochratoxin A (OTA), zearalenone (ZEA) and deoxynivalenol (DON) in vegetable oil by a modified QuEChERS approach, which was conventionally developed for pesticides analysis. A quick procedure of mycotoxins extraction and clean-up was achieved in two steps. Firstly, target analytes were extracted into the optimized solvent acetonitrile and followed by dispersive solid phase extraction (dSPE) clean up with the optimized sorbents to remove the co-extracts. Three types of d-SPE sorbents; C18, primary secondary amine (PSA) and graphitized carbon black (GCB) and four combination ratios of two selected d-SPEs were evaluated to achieve an optimum and acceptable result. The maximum co-extracts were removed when d-SPE C18 and GCB were used at ratio 3:1 with MgSO4 anhydrous followed by LC-MS/MS analysis, using an electro spray-ionization interface (ESI). Methanol as an organic phase and formic acid (0.1%) with 5 mM ammonium acetate as a polar phase, with total run of 16 minutes and flow rate 300 µLmin-1 were applied. The validation study indicated the seven mycotoxins could be detected in the concentration range of 0.01 ngg-1 to650.17ngg-1 with correlation coefficient > 0.98. The limit of quantitation (LOQ) ranges from 0.04 ngg-1 to 2000 ngg-1. The recoveries were in the range of 87.9% to 106.6%. The repeatability and reproducibility of the analysis were within the acceptable level (0.5 – 1.3) for precision using HORRAT ratio. Significant matrix effect was compensated using the matrix matched calibration curves. After validation, the method was successfully applied to 25 vegetable oil samples including corn oil, palm oil and sunflower oil. ZEA, AFG2, AFG1 and AFB1 were among the detected mycotoxins. A new fast, cost efficient, sensitive and accurate assay method was successfully developed, validated and applied for the determination of seven mycotoxins in vegetable oils.
format	Thesis
qualification_level	Master's degree
author	Kuppan, Sharmili
author_facet	Kuppan, Sharmili
author_sort	Kuppan, Sharmili
title	Method development for determination of multi-mycotoxin in vegetable oil using QuEChERS technique and liquid chromatography tandem mass spectrometry
title_short	Method development for determination of multi-mycotoxin in vegetable oil using QuEChERS technique and liquid chromatography tandem mass spectrometry
title_full	Method development for determination of multi-mycotoxin in vegetable oil using QuEChERS technique and liquid chromatography tandem mass spectrometry
title_fullStr	Method development for determination of multi-mycotoxin in vegetable oil using QuEChERS technique and liquid chromatography tandem mass spectrometry
title_full_unstemmed	Method development for determination of multi-mycotoxin in vegetable oil using QuEChERS technique and liquid chromatography tandem mass spectrometry
title_sort	method development for determination of multi-mycotoxin in vegetable oil using quechers technique and liquid chromatography tandem mass spectrometry
granting_institution	Universiti Putra Malaysia
publishDate	2015
url	http://psasir.upm.edu.my/id/eprint/65744/1/FSTM%202015%2032IR.pdf
_version_	1747812366106492928

Method development for determination of multi-mycotoxin in vegetable oil using QuEChERS technique and liquid chromatography tandem mass spectrometry

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