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Determination of Pesticide Residues in Mango Matrices by Ultra High-Performance Liquid Chromatography Coupled with Quadrupole Time-of-Flight Mass Spectrometry

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Abstract

This study describes an accurate mass measurement of pesticide residues (n = 68) in mango matrices by liquid chromatography coupled with quadrupole time of flight mass spectrometry (UHPLC-Q-TOF/MS). The proposed methodology is based on liquid-liquid extraction with a mixture of 25:75 (v/v) acetonitrile/ethyl acetate followed by dispersive solid phase extraction cleanup (primary secondary amine). Method validation was performed in order to establish accuracy, precision, matrix effect, limit of detection, and limit of quantification. The recoveries at three concentration levels (10, 50, and 100 μg kg−1) were in the range of 70–122% with intra- and inter-day relative standard deviations which were lower than 16%. The detection and quantification limits ranged from 0.5 to 7 μg kg−1 and from 2 to 25 μg kg−1, respectively. The developed method provides good linearity, accuracy, precision, and less matrix effects for the quantitation of selected pesticides. The study confirms that this analytical method can be routinely applied for the analysis of pesticide residues in mango matrices. Finally, the validated method was successfully applied to real samples and no positive samples were found.

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References

  • Abd-Alrahman SH (2014) Residue and dissipation kinetics of thiamethoxam in a vegetable-field ecosystem using QuEChERS methodology combined with HPLC-DAD. Food Chem 159:1–4

    Article  CAS  Google Scholar 

  • Bakırcı GT, Hışıl Y (2012) Fast and simple extraction of pesticide residues in selected fruits and vegetables using tetrafluoroethane and toluene followed by ultrahigh-performance liquid chromatography/tandem mass spectrometry. Food Chem 135:1901–1913

    Article  Google Scholar 

  • Banerjee K, Oulkar DP, Dasgupta S, Patil SB, Patil SH, Savant R et al (2007) Validation and uncertainty analysis of a multi-residue method for pesticides in grapes using ethyl acetate extraction and liquid chromatography–tandem mass spectrometry. J Chromatogr A 1173:98–109

    Article  CAS  Google Scholar 

  • Banerjee K, Oulkar DP, Patil SB, Jadhav MR, Dasgupta S, Patil SH, Bal S, Adsule PG (2009) Multi-residue determination and uncertainty analysis of 87 pesticides in mango by liquid chromatography tandem mass spectrometry. J Agri Food Chem 57:4068–4078

    Article  CAS  Google Scholar 

  • Bayarri S, Mart M, Carboneel I, Costel E (2012) Identifying drivers of liking for commercial spreadable cheeses with different fat content. J Sens Stud 27:1–11

    Article  Google Scholar 

  • Botero-Coy AM, Marin JM, Ibanez M, Sancho JV, Hernandez F (2012) Multi-residue determination of pesticides in tropical fruits using liquid chromatography/tandem mass spectrometry. Anal Bioanal Chem 402:2287–2300

    Article  CAS  Google Scholar 

  • Botitsi HV, Garbis SD, Economou A, Tsipi DF (2011) Current mass spectrometry strategies for the analysis of pesticides and their metabolites in food and water matrices. Mass Spectrom Rev 30:907–939

    CAS  Google Scholar 

  • Bruzzoniti MC, Checchini L, De Carlo RM, Orlandini S, Rivoira L, Del Bubba M (2014) QuEchERS sample preparation for the determination of pesticides and other organic resides in environmental matrices: a critical review. Anal Bioanal Chem 406:4089–4116

    Article  CAS  Google Scholar 

  • Cadena RS, Cruz AG, Netto RR, Castro WF, Faria JAF, Bolini HMA (2013) Sensory profile and physicochemical characteristics of mango nectar sweetened with high intensity sweeteners throughout storage time. Food Res Int 54:1670–1679

    Article  CAS  Google Scholar 

  • Deme P, Upadhyayula VV (2015) Ultra performance liquid chromatography atmospheric pressure photoionization high resolution mass spectrometric method for determination of multiclass pesticide residues in grape and mango juices. Food Chem 173:1142–1149

    Article  CAS  Google Scholar 

  • Di Stefano V, Avellone G, Bongiorno D, Cunsolo V, Muccilli V, Sforza S et al (2012) Applications of liquid chromatography–mass spectrometry for food analysis. J Chromatogr A 1259:74–85

    Article  CAS  Google Scholar 

  • Diez C, Traag WA, Zommerb P, Marinero P, Atienza J (2006) Comparison of an acetonitrile extraction/partitioning and “dispersive solid-phase extraction” method with classical multi-residue methods for the extraction of herbicide residues in barley samples. J Chromatogr A 113:11–23

    Article  Google Scholar 

  • Ferrer I, Thurman EM (2007) Multi-residue method for the analysis of 101 pesticides and their degradates in food and water samples by liquid chromatography/time-of-flight mass spectrometry. J Chromatogr A 1175:24–37

    Article  CAS  Google Scholar 

  • Ferrer I, Garcia-Reyes JF, Fernandez-Alba A (2005) Identification and quantitation of pesticides in vegetables by liquid chromatography time of-flight mass spectrometry. Trends Anal Chem 24:671–682

    Article  CAS  Google Scholar 

  • Ferrer CA, Lozano A, Agüera A, Jiménez Fernández AR (2011) Overcoming matrix effects using the dilution approach in multiresidue methods for fruits and vegetables. J Chromatogr A 1218:7634–7639

    Article  CAS  Google Scholar 

  • Filho AM, dos Santos FN, Pereira PA (2011) Multi-residue analysis of pesticide residues in mangoes using solid-phase micro extraction coupled to liquid chromatography and UV-Vis detection. J Sep Sci 34:2960–2960

    Article  CAS  Google Scholar 

  • Fleury Filho N, Nascimento CA, Faria EO, Cruvinel AR, Oliveira JM (2012) Within-laboratory validation of a multi residue method for the analysis of 98 pesticides in mango by liquid chromatography tandem mass spectrometry. Food Addit Contam Part A Chem Anal Control Expo Risk Assess 29:641–656

    Article  CAS  Google Scholar 

  • Fontana AR, Rodriguez I, Ramil M, Altamirano JC, Cela R (2011) Liquid chromatography time-of-flight mass spectrometry follows sorptive micro extraction for the determination of fungicide residues in wind. Anal Bioanal Chem 401:767–775

    Article  CAS  Google Scholar 

  • Gomez-Ramos MM, Ferrer C, Malato O, Aguera A, Fernandez-Alba AR (2013) Liquid chromatography-high-resolution mass spectrometry for pesticide residue analysis in fruit and vegetables: screening and quantitative studies. J Chromatogr A 1287:24–37

    Article  CAS  Google Scholar 

  • González-Curbelo MA, Socas-Rodríguez B, Herrera-Herrera AV, González-Sálamo J, Hernández-Borges J, Rodríguez-Delgado MA (2015) Evolution and applications of the QuEChERS method. Trends Analyt Chem 71:169–185

    Article  Google Scholar 

  • Grimalt S, Sancho JV, Pozo OJ, Hernandez F (2010) Quantification confirmation and screening capability of UHPLC coupled to triple quadrupole and hybrid quadrupole time-of-flight mass spectrometry in pesticide residue analysis. J Mass Spectrom 45:421–436

    CAS  Google Scholar 

  • Hernandez F, Pozo OJ, Sancho JV, Lopez FJ, Marın JM, Ibanez M (2005) Strategies for quantification and confirmation of multi-class polar pesticides and transformation products in water by LC-MS2 using triple quadrupole and hybrid quadrupole time of flight analyzers. Trends Anal Chem 24:596–612

    Article  CAS  Google Scholar 

  • Hiemstra M, Kok A (2007) Comprehensive multi-residue method for the target analysis of pesticides in crops using liquid chromatography–tandem mass spectrometry. J Chromatogr A 1154:3–25

    Article  CAS  Google Scholar 

  • Lehotay SJ (2011) QuEChERS sample preparation approach for mass spectrometric analysis of pesticide residues in foods. Methods Mol Biol 747:65–91

    Article  CAS  Google Scholar 

  • Liu G, Rong L, Guo B, Zhang M, Li S, Wu Q et al (2011) Development of an improved method to extract pesticide residues in foods using acetontrile with magnesium sulfate and chloroform. J Chromatogr A 1218:1429–1436

    Article  CAS  Google Scholar 

  • Malik AK, Blasco C, Pico Y (2010) Liquid chromatography-mass spectrometry in food safety. J Chromatogr A 1217:4018–4040

    Article  CAS  Google Scholar 

  • Martinez Vidal JL, Fernandez Moreno JL, Arrebola Liebanas FJ, GarridoFrenich A (2007) Application of low-pressure gas chromatography/tandem mass spectrometry to the determination of pesticide residues in tropical fruits. J AOAC Int 90:1146–1164

    Google Scholar 

  • Martinez R, Torres P, Meneses MA, Figueroa JG, Perez-Alvarez JA, Viuda Martos M (2012) Chemical, technological and in vitro antioxidant properties of mango, guava, pineapple and passion fruit dietary fiber concentrate. Food Chem 135:1520–1526

  • Mokarizadeh A, Faryabi MR, Rezvanfar MA, Abdollahi M (2015) A comprehensive review of pesticides and the immune dys regulation: mechanisms evidence and consequences. Toxicol Mech Methods 25:258–278

    Article  CAS  Google Scholar 

  • Moretto A, Colosio C (2011) Biochemical and toxicological evidence of neurological effects of pesticides: the example of Parkinson’s disease. Neurotoxicology 32:383–391

    Article  CAS  Google Scholar 

  • Navickiene S, Aquino A, Bezerra DS (2010) A matrix solid-phase dispersion method for the extraction of seven pesticides from mango and papaya. J Chromatogr Sci 48:750–754

    Article  CAS  Google Scholar 

  • Pico Y, Blasco C, Farre M, Barcelo D (2009) Analytical utility of quadrupole time-of-flight mass spectrometry for the determination of pesticide residues in comparison with an optimized column high performance liquid chromatography/tandem mass spectrometry method. J AOAC Int 92:734–744

    CAS  Google Scholar 

  • Ribeiro SMR, Barbosa LCA, Queiroz JH, Kno M, Schieber A (2008) Phenolic compounds and antioxidant capacity of Brazilian mango (Mangifera indica L.) varieties. Food Chem 110:620–626

    Article  CAS  Google Scholar 

  • SANTE (2015) Guidance document on analytical quality control and validation procedures for pesticide residues analysis in food and feed directorate general health and consumer protection, European Commission. SANTE/11945/2015

  • Savant RH, Banerjee K, Utture SC, Patil SH, Dasgupta S, Ghaste MS, Adsule PG (2010) Multiresidue analysis of 50 pesticides in grape pomegranate and mango by gas chromatography ion trap mass spectrometry. J Agri Food Chem 58:1447–1454

    Article  CAS  Google Scholar 

  • Sharma D, Nagpal A, Pakade YB, Katnoria JK (2010) Analytical methods for estimation of organophosphorus pesticide residues in fruits and vegetables: a review. Talanta 82:1077–1089

    Article  CAS  Google Scholar 

  • Shelton JF, Geraghty EM, Tancredi DJ, Delwiche LD, Schmidt RJ, Ritz B, Hansen RL, Hertz-Picciotto I (2014) Neurodevelopmental disorders and prenatal residential proximity to agricultural pesticides: the charge study. Environ Health Perspect 122:1103–1109

    Google Scholar 

  • Sinha SN, Bhatnagar VK, Doctor P, Toteja GS, Agnihotri NP, Kalra RL (2011) A novel method for pesticide analysis in refined sugar samples using a gas chromatography-mass spectrometer (GC-MS/MS) and simple solvent extraction method. Food Chem 126:379–386

    Article  CAS  Google Scholar 

  • Sinha SN, Vasudev K, Vishnu Vardhana Rao M (2012) Quantification of organophosphate insecticides and herbicides in vegetable samples using the “Quick Easy Cheap Effective Rugged and Safe” (QuEChERS) method and a high performance liquid chromatography-electrospray ionization-mass spectrometry (LC–MS/MS) technique. Food Chem 132:1574–1584

    Article  CAS  Google Scholar 

  • Sivaperumal P, Anand P, Riddhi L (2015) Rapid determination of pesticide residues in fruits and vegetables using ultra-high-performance liquid chromatography/time-of-flight mass spectrometry. Food Chem 168:356–365

    Article  CAS  Google Scholar 

  • Soler C, James KJ, Pico Y (2007) Capabilities of different liquid chromatography tandem mass spectrometry systems in determining pesticide residues in food application to estimate their daily intake. J Chromatogr A 1157:73–84

    Article  CAS  Google Scholar 

  • Stachniuk A, Fornal E (2016) Liquid chromatography-mass spectrometry in the analysis of pesticide residues in food. Food Anal Method 9:1654–1665

    Article  Google Scholar 

  • Starks SE, Gerr F, Kamel F, Lynch CF, Alavanja MC, Sandler DP, Hoppin JA (2012) High pesticide exposure events and central nervous system function among pesticide applicators in the Agricultural Health Study. Int Arch Occup Environ Health 85:505–515

    Article  CAS  Google Scholar 

  • Wang J, Leung D (2009) Applications of ultra-performance liquid chromatography electrospray ionization quadrupole time-of-flight mass spectrometry on analysis of 138 pesticides in fruit- and vegetable based infant foods. J Agri Food Chem 57:2162–2173

    Article  CAS  Google Scholar 

  • Wang X, Wang S, Cai Z (2013) The latest developments and applications of mass spectrometry in food-safety and quality analysis. Trends Anal Chem 52:170–185

    Article  CAS  Google Scholar 

  • Wong JW, Zhang K, Hayward DG, Kai-Meng C (2011) Multiresidue pesticide analysis by capillary gas chromatography–mass spectrometry. Methods Mol Biol 747:131–172

    Article  CAS  Google Scholar 

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Acknowledgements

The authors are grateful to the Director, National Institute of Occupational Health, Ahmedabad, for granting permission to publish the article. The authors acknowledge the Indian Council of Medical Research for the financial assistance of the project (IRIS ID No. 2011-02530).

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Correspondence to P. Sivaperumal.

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P. Sivaperumal declares that he/she has no conflict of interest. A. Salauddin declares that he/she has no conflict of interest. A. Ramesh Kumar declares that he/she has no conflict of interest. K. Santhosh declares that he/she has no conflict of interest. T. Rupal declares that he/she has no conflict of interest.

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Sivaperumal, P., Salauddin, A., Ramesh Kumar, A. et al. Determination of Pesticide Residues in Mango Matrices by Ultra High-Performance Liquid Chromatography Coupled with Quadrupole Time-of-Flight Mass Spectrometry. Food Anal. Methods 10, 2346–2357 (2017). https://doi.org/10.1007/s12161-016-0779-9

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