Determination of Target Pesticide Residues in Tropical Fruits Employing Matrix Solid-Phase Dispersion (MSPD) Extraction Followed by High Resolution Gas Chromatography

Abstract

A simple method based on matrix solid-phase dispersion (MSPD) extraction and gas chromatography with electron-capture detection (GC-ECD) is employed to determine pesticide residues in the following tropical fruits: banana, mango, melon, papaya and pineapple. In the MSPD proposed method, C18, silica gel and ethyl acetate presented the best results in the extraction, clean-up and elution steps, respectively. Spiked blank samples were used to minimize the matrix effect in the chromatographic determination. The validation process was conducted at three different concentration levels of spiked samples (0.50-2.50 µg g -1 ) in within-a-day and in among days assays. The limits of detection for the pesticides ranged from 4.0 to 23 µg kg -1 . The method showed acceptable selectivity, coefficients of correlation higher than 0.997, and recovery between 76-105%. The within-a-day precision was assessed through the relative standard deviation (2.8-19%) for the different levels of spiked samples tested.Keywords: matrix solid-phase dispersion, pesticide residues, method validation, GC-ECD IntroductionThe recent Brazilian fruit growing jumped the country to an important position in the international agribusiness sector. In 2015, Brazil set a record in fruit exports with a total fresh fruit sales achieving US$ 735 million, a performance around US$ 100 million higher than 2014. With a variety of crops produced throughout the country and in different climates, Brazil is the leading world producer of oranges; the secondleading producer of bananas and papayas; the third-largest producer of pineapples; and an important producer of Tahiti lemons, tangerines and grapes. 1 Brazil is, after China and India, the third largest producer of fruit in the world (43 million ton per year). About 70% of Brazil's fruit exports go to Europe and the overarching goal of Brazilian fruit cultivation is to consolidate its position as the leader in the international market. Approximately 711,000 tons of the Brazilian fruits are exported to more than 110 countries being mangoes, melons, oranges, grapes, papayas, limes and bananas the main fruits exported in 2014. According to the Brazilian association of producers and exporters of fruit, the country has conditions to reach US$ 1 billion in exports of fresh fruit by 2017 if it can conform to international phytosanitary and customs conditions through better control of domestic production. 1The international market has strongly signaled that there is a movement of consumers looking for healthy food and without agrochemical residues considered to be harmful to human health. The European Community, mainly, have required that the exporters take into account the respect with the environment, traceability and working conditions, health of workers involved in food production and level of pesticide residues.The European Union and the United Kingdom banned mangoes imported from India until the country meets the phytosanitary standards that will ensure they are pest-free. 2,3The entrance of cherries from countri...

Comparison of gas chromatography detectors and its application in food analysis

“…ECD is a detector that can detect electron affine compounds due to high sensitivity and selectivity to high electronegative compounds (Scott, 1996). This detection used hydrogen as carrier gas and can be used to analyse the pesticide and residue in fruits and vegetables with high water content, also fish (Stocka, et al, 2016;Farina, et al, 2017;Yousefi, et al, 2017;Lukyanova, et al, 2018;Freitas, et al, 2018). In food analysis, ECD could be used to detect volatile compounds in beer (da Silva, et al, 2015), and analyze metabolites in sugarcane (Biswas, et al, 2019).…”

Achievements and Challenges of Matrix Solid-Phase Dispersion Usage in the Extraction of Plants and Food Samples

“…Taking into account the above-mentioned phenomena, matrix solid-phase dispersion (MSPD) is one of the methods that apply the extraction of analytes in the liquid-solid system [10][11][12][13][14][15][16][17]. The MSPD method has been widely used in the sample preparation, extraction, and fractionation of solid, semi-solid, and/or highly viscous biological samples.…”

“…After homogenization, the mixture is transferred to an SPE column where it is eluted with an appropriate eluent (a single organic solvent or a mixture). The MSPD application range is broad and it can thus be employed to perform the simultaneous extraction of numerous compounds from various matrices, e.g., essential oils from herbs [10], catechins and alkaloids from green tea leaves [11], rutin from black elderberry [12], phenolic compounds from tea fruit [13], pesticides from fruits [14][15][16], and free fatty acids from chocolate [17].…”

Ανάπτυξη Αναλυτικών Μεθόδων Προσδιορισμού Παρασιτοκτόνων Σε Ιχθυοκαλλιέργειες Και Εκτίμηση Επικινδυνότητας

“…Πρόκειται για μία εύχρηστη τεχνική, φιλικής προς το περιβάλλον, λόγω των μικρών ποσοτήτων οργανικών διαλυτών που χρησιμοποιούνται, με μικρούς χρόνους ανάλυσης. Έχει αποδειχτεί ότι είναι πολύ αποτελεσματική στην εκχύλιση φυτοφαρμάκων, πολυκυκλικών αρωματικών υδρογονανθράκων (PAHs) και κτηνιατρικών φαρμάκων σε υποστρώματα όπως οικιακή σκόνη, λαχανικά, δημητριακά, τρόφιμα ζωικής προέλευσης, φρούτα, γάλα, αυγά και ψάρια (Balsebre et al, 2018;Freitas et al, 2018;Nardelli et al, 2018;Soares et al, 2017και Zhao et al, 2018. Σχήμα 3.12: Τεχνική εκχύλιση με διασπορά υποστρώματος σε στερεά φάση…”