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Comparative Evaluation of QuEChERS Method Coupled to DLLME Extraction for the Analysis of Multiresidue Pesticides in Vegetables and Fruits by Gas Chromatography-Mass Spectrometry

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Abstract

An economical and rapid multiresidue method has been developed using quick, easy, cheap, effective, rugged and safe (QuEChERS) procedure combined with dispersive liquid-liquid microextraction (DLLME) for the quantitative determination of 36 multiclass, multiresidue pesticides (13 organochlorines, 11 organophosphates, and 12 synthetic pyrethroids) in different vegetables and fruits without primary and secondary amine (PSA) cleanup step followed by gas chromatography-mass spectrometry (GC-MS) analysis. The procedure mainly involves the acetonitrile extraction in the presence of anhydrous MgSO4 and NaCl followed by DLLME using carbon tetrachloride (extraction solvent) and acetonitrile (disperser solvent). Experimental parameters were optimized using design of experiments (DoE) approach. The method developed without PSA cleanup step has yield similar analytical performance with that of method with PSA cleanup step for all the pesticides analyzed. The precision of the developed method was found to be less than 12 % and limit of detection for all the analyzed pesticides was found to be in the range of 0.001–0.010 mg kg−1. This method was successfully applied in different fruits and vegetables and the recoveries were found to be in the range of 87–106 % at 0.05 mg kg−1 with an acceptable precision (<16 %). Coupling of QuEChERS with DLLME may be an appropriate replacement to eliminate costly PSA and makes the QuEChERS method more economical, time saving, without losing its analytical efficiency. The samples collected from Lucknow City, India, were analyzed for the presence of pesticides and only three pesticides β-cypermethrin, λ-cyhalothrin, and chlorpyrifos were found to have value above PFA-1954/CODEX-MRL values. The method has immense utility to use it for routine analysis of multiclass, multiresidue pesticides in fruits and vegetables.

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Acknowledgments

The authors are grateful to Prof. Alok Dhawan, Director, CSIR-Indian Institute of Toxicology Research, Lucknow, for his keen interest and support to provide infrastructural facilities to carry this work. Manuscript bears CSIR-IITR communication no. 3334.

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Authors and Affiliations

  1. Pesticide Toxicology Laboratory, Regulatory Toxicology Group, CSIR-Indian Institute of Toxicology Research (CSIR-IITR), MG Marg, Lucknow, Uttar Pradesh, 226001, India

    Satyajeet Rai, Abhishek Kumar Singh, Anshuman Srivastava, Sapna Yadav & Mohana Krishna Reddy Mudiam

  2. Department of Bioengineering, Faculty of Engnieering, Integral University, Lucknow, Uttar Pradesh, 226026, India

    Satyajeet Rai & Mohammed Haris Siddiqui

  3. Analytical Chemistry Laboratory, Regulatory Toxicology Group, CSIR-Indian Institute of Toxicology Research (CSIR-IITR), MG Marg, Lucknow, Uttar Pradesh, 226001, India

    Mohana Krishna Reddy Mudiam

  4. Mass & Analytical (NCMS) Division, CSIR-Indian Institute of Chemical Technology, Tarnaka, Uppal Road, Hyderabad, 500 007, India

    Mohana Krishna Reddy Mudiam

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  1. Satyajeet Rai
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  2. Abhishek Kumar Singh
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  3. Anshuman Srivastava
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  4. Sapna Yadav
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  5. Mohammed Haris Siddiqui
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  6. Mohana Krishna Reddy Mudiam
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Correspondence to Mohana Krishna Reddy Mudiam.

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This study was funded by CSIR, New Delhi (BSC0111, INDEPTH).

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Rai, S., Singh, A.K., Srivastava, A. et al. Comparative Evaluation of QuEChERS Method Coupled to DLLME Extraction for the Analysis of Multiresidue Pesticides in Vegetables and Fruits by Gas Chromatography-Mass Spectrometry. Food Anal. Methods 9, 2656–2669 (2016). https://doi.org/10.1007/s12161-016-0445-2

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