30 Environmental Laboratory
DEVELOPMENT OF ANALYTICAL METHODS TO ASSESS ANTIMICROBIAL CONTAMINATION IN THE ENVIRONMENT AND ITS TRANSFER IN THE FOOD CHAIN
The extensive use of antimicrobials (AMs) in agriculture has led to the occurrence of residual drugs in diff erent environmental matrices such as animal manure (Zalewska et al., 2021), soils (Hang et al., 2021) and vegetables (Kang et al., 2013) frequently consumed by humans, among others. This could pose a potential threat to human health, not only because of the possible eff ects after ingestion but also because the transmission of AM-resistant genes could occur (Jadeja & Worrich, 2022).
I
n this sense, two accurate sample preparation procedures were developed and validated for the simultaneous analysis of sulfonamides (SAs) and tetracyclines (TCs) in four of the most widely consumed vegetables (lettuce, onion, tomato, and carrot) in Europe (Vergara-Luis, Báez-Millán, et al., 2023). The evaluated protocols were based on QuECHERS (Quick, Easy, Cheap, Effective, Rugged and Safe) for extraction and subsequent clean- up by SPE (solid phase extraction) or dispersive SPE. Parameters affecting both extraction and clean-up were carefully evaluated and selected for accuracy of results and minimal matrix effect (Figure 1).
Overall, apparent recoveries were above 70 % for most of the target analytes with both analytical procedures, and adequate precision (RSD < 30 %) was obtained for all the matrices. The procedural limits of quantifi cation (LOQPRO
remained below 4.4 μg·kg-1 chlortetracycline (CTC) in lettuce (11.3 μg·kg-1
) values for SPE clean-up
for TCs in all vegetables except for ) and 3.0 μg·kg-1
). Lower LOQPRO for
SAs, with the exception of sulfadiazine (SDZ) in onion (3.9 μg·kg-1 and sulfathiazole (STZ) in carrot (5.0 μg·kg-1 (0.1-3.7 μg·kg-1
) were obtained, in general, when dSPE clean-up
was employed. Both methods were applied to twenty-fi ve market vegetable samples from ecological and conventional agriculture and only sulfamethazine (SMZ) and sulfapyridine (SPD) were detected in lettuce at 1.2 μg·kg-1
and 0.5 μg·kg-1 , respectively.
Moreover, an accurate analytical method was also developed for the simultaneous analysis of twenty-four AMs in soil:compost and animal manure samples by means of Ultra-High Performance Liquid Chromatography coupled to a triple-quadrupole mass spectrometer (UHPLC-QqQ) (Vergara-Luis, Bocayá, et al., 2023).
Figure 1. Matrix effect (ME) % (n=3) at the detection for the target analytes in the four vegetable matrices with SPE and dSPE clean-up approaches. ) values
AET ANNUAL BUYERS’ GUIDE 2024
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