Abstract

In this study two analytical methods, one based on matrix solid phase dispersion (MSPD) and the other on liquid–solid extraction (LSE), coupled with gas chromatography, were evaluated and used to determine the presence of 163 pesticides (6 acaricides, 62 fungicides, 18 herbicides and 77 insecticides) in various herbs. Both methods were optimized considering different parameters (sample to sorbent mass ratio, extracting solvent, sorbents for clean-up step, etc.). The results of these validated sample preparation procedures were compared. Under optimum conditions, the mean recoveries obtained were in the range of 70–119 % for MSPD for most pesticides and 70–118 % for LSE, but with several exceptions. Precision values, expressed as relative standard deviation (RSD), were ≤16 % for MSPD and <18 % for LSE. Correlation coefficients were higher than 0.99254 for both methods. LODs (limits of detection) and LOQs (limits of quantification) for MSPD were within the ranges of 0.003–0.03 and 0.005–0.04 mg/kg, respectively. The data demonstrate that the MSPD method was successfully used for the analysis of 163 pesticides in the following herbs: chamomile (Matricaria chamomilla L.), linden (Tilia), lungwort (Pulmonaria L.), melissa (Melissa L.), peppermint (Mentha piperita L.) and thyme (Thymus vulgaris L.). This paper indicates the potential of MSPD for qualitative and quantitative analysis of pesticide residues. This method was therefore validated at three spiking levels (the first ranging from 0.005 to 0.05 mg/kg, the second from 0.05 to 0.5 mg/kg and the third from 0.25 to 2.5 mg/kg) and applied to real samples (n = 15). MSPD proves to be a simple, fast and very useful multiresidue method and can be recommended for routine pesticide monitoring studies in various herbs.

Highlights

  • Herbs play an important role in our health and our food and have a variety of culinary and medicinal uses

  • The data demonstrate that the matrix solid phase dispersion (MSPD) method was successfully used for the analysis of 163 pesticides in the following herbs: chamomile (Matricaria chamomilla L.), linden (Tilia), lungwort (Pulmonaria L.), melissa (Melissa L.), peppermint (Mentha piperita L.) and thyme (Thymus vulgaris L.)

  • The main objective of this work was to optimize the process of preparation, extraction and purification of herbal samples using MSPD and liquid–solid extraction (LSE) for qualitative and quantitative analysis of a wide spectrum of pesticide residues

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Summary

Introduction

Herbs play an important role in our health and our food and have a variety of culinary and medicinal uses. Herbs have been in use in the human diet and traditional medicine since antiquity, they have recently become the center of attention of the nutrition-science world because of their potential health benefits and detoxification properties. There are many herbal benefits: they have hypotensive or antihypertensive effects [1, 2] and contain unique antioxidants [3], essential oils, vitamins, phytosterols and many other plant-derived nutrients, which help the immune system defend the body against viruses, toxins, bacteria and other germs [4]. Medicinal plants and herbal materials may be found with various kinds of microbial contaminants, of which bacterial and fungal infections are regarded as the most common [5]. Herbs may be contaminated by toxic chemical substances such as mycotoxins, heavy metals, pesticides and deposited pesticide residues.

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