Residue Levels Research Articles

Waste and residue management: sustainable hospital catering services

ObjectiveHospital catering services, like other food and beverage businesses, have the potential to cause negative environmental impacts. This study aims to analyze the food waste, food residue, and non-food waste calculations of the menus used in hospital catering services.MethodThe study was conducted in all 4 seasons and 31 day months were included in the study to standardize the number of days of practice in the selection of seasonal menus. In the menus, one of the most frequently produced dishes using traditional production methods was selected separately for lunch and dinner. In the study, food waste, food residue, and non-food waste calculations of pre-selected meals applied in hospital catering services were made.ResultsIn the spring, summer, autumn, and winter seasons, the food waste levels of the one portion for the first group were significantly higher than the food waste levels of the second group and one portion for the third group (p < 0.001). In the summer season, the level of food residue of one portion for the second group was significantly higher than the level of food residue of one portion for the first group (p < 0.05). In all seasons, the levels of non-food waste of one portion for the second group were significantly lower than the levels of non-food waste of the first group and one portion for the third group (p < 0.05).ConclusionDietitians need to plan menus by adopting sustainable nutrition models. In this context, efforts should be made to plan menus in which local suppliers will be supported and food waste and non-food waste will be reduced. In-service training activities covering strategies and activities to reduce food waste and food residues should be planned for kitchen and service personnel under the leadership of food services and nutrition dietitians.

Effects of cereal rye residue biomass and preemergence herbicide on the emergence of troublesome southeastern weed species

Cover crops are increasingly adopted to suppress weed growth and reduce reliance on chemical herbicides. A greenhouse experiment was conducted to evaluate the emergence and growth response of troublesome southeastern weeds to various cereal rye (Secale cereale L.) residue levels. Trays planted with Palmer amaranth (Amaranthus palmeri S. Watson), sicklepod (Senna obtusifolia L.), ivyleaf morningglory (Ipomoea hederacea), and large crabgrass (Digitaria sanguinalis L.) seeds mixed with soil were covered uniformly by four different levels of cereal rye biomass. The following field experiment was conducted at two locations in Alabama in a split-plot design, with the main plot factor being four seeding rates of cereal rye to obtain various cereal rye biomass. Subplot factors were preemergence herbicide flumioxazin and non-treated (NT) check. The greenhouse results demonstrated reduced seed emergence and lower weed biomass for Palmer amaranth, sicklepod, and large crabgrass in plots with higher cereal rye residue biomass compared to those with lower biomass. In both greenhouse and field conditions, the emergence of ivyleaf morningglory was not affected by the increasing biomass of cereal rye residue. Palmer amaranth seed emergence was the most sensitive to increasing biomass residue due to its small seed size. Cereal rye biomass and Palmer amaranth counts were strongly negatively correlated with a Pearson’s coefficient (r) of 0.83 while weakly negatively correlated for ivyleaf morningglory with 0.49. In conclusion, increasing the biomass of cereal rye residue is effective in suppressing Palmer amaranth seed emergence but not ivyleaf morningglory. The flumioxazin treatment demonstrated 95%–90% control for Palmer amaranth and ivyleaf morningglory, while the NT check exhibited 50% control of Palmer amaranth and 30% control of ivyleaf morningglory by cereal rye biomass alone. In conclusion, a sufficient amount of cereal rye biomass can effectively suppress the emergence and growth of weeds, particularly Palmer amaranth.

Understanding factors that affect dislodgeable foliar residues of pyrimethanil and their dissipation: How relevant is the crop-type for human exposure?

Pesticide dislodgeable foliar residues (DFR) and their dissipation half-time (DT50) after application are important parameters for exposure and risk assessment from intended reentry activities or unintended dermal contact with treated crops. To understand the impact of agronomic factors on residue level a statistical based evaluation was conducted using ten DFR studies, with pyrimethanil applied in Scala® to strawberries, raspberries, peppers, apples, and grapes, 30 trials in total. Influences on initial DFR (DFR0) and DT50 were investigated by multivariate linear regression analysis. The application rate and the crop itself indicate a potential influence on DFR0 when related to ground area applied which is not notable for three dimensional crops regardless of indoor/outdoor cultivation, when related to leaf wall area (LWA). DFR0 values for pyrimethanil do not depend on the number of applications as the range of DT50 values determined for pyrimethanil is consistently small (0.3–2.3 days). All DT50 are significantly lower than the European default (30 days). The noted difference in DT50 of peppers to strawberries is likely attributable to indoor cultivation. A proposal is made how to refine the exposure assessment of pyrimethanil making use of the available DFR0 and DT50 data for other crop types.

Quantum Dots‐Engineered Flexible Hydrogel as Plant‐Wearable Sensor for on‐Site Profiling Dynamic Pesticide Degradation

AbstractEngineering wearable devices for in situ and on‐site monitoring of pesticide residues from plants in a non‐destructive manner is of great research value but remains a huge challenge. In this study, a plant‐wearable fluorescence sensor CdTe CDs@PVA@AG, is designed and constructed by embedding CdTe QDs in polyvinyl alcohol (PVA) and agarose (AG)‐co‐assembled double‐network hydrogel to transmit on‐the‐scene pesticides residues messages. Harnessing red emission and stimuli‐responsive performance of CdTe QDs, as well as hydrogel's excellent flexibility, high adhesion, and porous network, CdTe CDs@PVA@AG is endowed with quantitative response to thiram at ≈µm level within 2 min through promoting fluorescence silence in conjunction with the transformation of images into primary colors as digital signals. More interestingly, CdTe CDs@PVA@AG is capable of being tightly pasted onto various crops’ surfaces and then is not only explored to appraise pesticide residue levels but also to profile the dynamic pesticide degradation, in a non‐destructive manner. This work opens up a new avenue to engineer plant‐wearable devices for in situ, on‐site, and non‐destructive capturing of the pesticide residue information from crops, favoring the accurate monitoring of the health status of crops, and rapid and healthy development of smart agriculture.

The rhizosphere bacteriome is modified by wheat genotype and growth stage under increased imidazolinone herbicide residues

Abstract When imidazolinone herbicides persist longer than intended and remain active in the soil, they can have unknown impacts on soil health. This study investigated the impact of simulated soil residues of an imidazolinone herbicide on shoot dry matter and bacterial communities in the bulk and rhizosphere soil in tolerant and susceptible wheat genotypes, at two different crop growth stages. Four levels of gradient increased herbicide residues were applied, and rhizosphere bacterial diversity and community composition were analysed using 16S rRNA gene amplicon sequencing. Our results highlight that the shift in wheat rhizosphere bacteriome is driven more by the crop growth stage and wheat genotype than the presence and level of imidazolinone residues. Results showed a linear trend of increasing alpha diversity with increasing herbicide residues during the early crop growth stage, and a decrease in alpha diversity with increasing herbicide residues during the late crop growth stage, only for the tolerant genotype. The order Betaproteobacteriales in the rhizosphere was increased by herbicide residues to a greater extent than the other taxonomic groups. During the early growth stage, there were more ASV (amplicon sequence variant) enriched by imidazolinone herbicide residues in the rhizosphere of the tolerant genotype compared with the susceptible genotype. Future research work should consider studies with soils that have different physicochemical properties, and focus on other soil microbes of known significance to nutrient cycling and crop growth.

Influence of Eimeria spp. and Clostridium perfringens Infection on Growth Performance and Toltrazuril Residues in Chickens.

Coccidiosis and necrotic enteritis are among the most common diseases affecting poultry, with economic impact due to reduced production and the costs of treatment and prevention. Eimeria invasion contributes to gut damage that promotes the growth of other harmful pathogens, such as Clostridium perfringens. Coccidiostats, with toltrazuril as an example, are widely used to control these infections. In this study, we assessed the effects of Eimeria spp. infection and coinfection with Eimeria spp. and Clostridium perfringens on chicken weight and toltrazuril concentrations, along with two metabolites-toltrazuril sulfoxide and toltrazuril sulfone-using liquid chromatography coupled with mass spectrometry. The analysis of liver and muscle samples showed lower levels of residues in groups challenged with Eimeria spp. In the case of combined Eimeria and C. perfringens infection, no significant differences were observed. These findings suggest that the combination of Eimeria and C. perfringens does not significantly alter the residue levels of toltrazuril and its metabolites, providing valuable insight into the pharmacokinetics of toltrazuril in poultry under infection conditions. This research contributes to optimizing drug use and residue management in poultry production.

Antibiotic Residues in Animal Products from Some African Countries and Their Possible Impact on Human Health.

This review investigates the levels of antibiotic residues in animal products, types of antibiotics, and their possible impact on human health in Africa. The literature search involved the use of a systematic survey using data that were published from Africa from 2015 to 2024. The search terms used the Boolean operators with keywords such as antibiotics, antibiotic residues, antibiotics in animal products in Africa, and impact on human health. Only research conducted in Africa was used in the present study. The findings showed that the most prevalent groups of antibiotic residues were aminoglycoside, macrolides, β-lactams, fluoroquinolones, tetracyclines sulfonamides, and phenicols. Tetracycline showed the most prevalent antibiotic residue with 43% mostly from East Africa, followed by sulfonamides at 19%, and β-lactams at 16%; most of the antibiotic residue levels were higher than the World Health Organization permissible limit. Noncompliance with withdrawal periods and maximum residue limits for antibiotics used in food-producing animals may lead to negative outcomes such as allergic reactions, teratogenicity, carcinogenicity, microbiome alterations, and, most notably, antibiotic resistance. As a result, there is a need for constant monitoring of antibiotic residues in animal products in addition to the consideration of alternatives to antibiotics in order to avoid their health implications.

Pesticides in Honeybee Products-Determination of Pesticides in Bee Pollen, Propolis, and Royal Jelly from Polish Apiary.

The bioaccumulation of pesticides in honeybee products (HBPs) should be studied for a number of reasons. The presence of pesticides in HBPs can provide new data on the risk related to the use of pesticides and their role in bee colony losses. Moreover, the degree of contamination of HBPs can lower their quality, weaken their beneficial properties, and, in consequence, may endanger human health. The aim of this study was to quantify a broad range of pesticide residues in three different HBPs-bee pollen, propolis, and royal jelly. Samples were collected in the years 2017-2019 from the apiary in west-central Poland. Bee products were analyzed for the presence of over 550 pesticides using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) method. Twenty-nine of the contaminants were quantified at least in one of the samples. Nine of them exceeded the maximum residue levels for honey. It should be noted that any dose of pesticides can cause a health hazard due to toxicity, since these substances may act synergistically. This current study revealed the high need for the pesticide monitoring of HBPs and proved that there is a need to expand the European Union Pesticides Database to include more HBPs.

Detection of glyphosate, glufosinate, and their metabolites in multi-floral honey for food safety

Beehives can accumulate environmental contaminants as bees gather pollen, propolis, and water from their surroundings, contaminating hive products like honey. Moreover, in multifloral environments, bees can interact with plants treated with different pesticides, often causing higher pesticides concentrations in multi-floral honey than in mono-floral varieties. Glyphosate and glufosinate are both widely used herbicides. Glyphosate accounted for one-third of herbicide sales in Europe in 2017 and continues to raise health concerns, including its potential carcinogenicity. While the European Commission extended glyphosate’s authorisation for another 10 years in 2023, concerns remain about its impact on biodiversity and human health. This study aimed to monitor the presence of glyphosate, glufosinate, and their metabolites in 100 samples of multifloral honey representing Italian production by analysis using IC-HRMS. Results indicated that 12% of honey samples contained glyphosate residues ranging from > LOQ to 45 ng g−1, with the highest concentrations detected in the Puglia region. No sample exceeded the maximum residue levels set by EU regulations. Glufosinate and its metabolites were not detected in any samples. These findings underscore the need for continued monitoring of pesticide residues in honey, particularly given the potential ‘cocktail effect’ of multiple contaminants and their combined toxicity. This study highlights the importance of safeguarding consumer health, especially in vulnerable populations, by addressing gaps in data on pesticide residue levels.

Effect of Stir-Frying, Boiling, and Baking on Hexaconazole Residue Levels in Welsh Onion (Allium fistulosum L.).

Hexaconazole, a triazole insecticide, is widely used to control rust disease in Welsh onions. Residue levels of pesticides vary based on the cooking methods. Although studies on hexaconazole residue have involved vegetables such as cabbage, research on Welsh onion is limited. This study investigated the effect of different cooking methods on hexaconazole residues. Welsh onion was processed by common cooking methods such as stir-frying, boiling, and baking, and analyzed for pesticide residues using liquid chromatography with tandem mass spectrometry. The results showed that the removal rates of pesticides after cooking were 40.0-62.9% for stir-frying, 80.0-91.4% for boiling, and 51.4-77.1% for baking. Regardless of cutting thickness (0.8 cm or 5 cm), the reduction rate of pesticide residues increased with time during boiling. Increased reduction rates were also observed with increased time during baking. As stir-frying time increased, the residue amount increased due to water loss. However, the absolute amount of the pesticide decreased with increasing time. Therefore, the residue amount of hexaconazole in Welsh onion was reduced by various general cooking processes. These findings can provide a valuable foundation for research on Welsh onion processing, address consumer concerns about pesticide residues, and provide baseline data for risk assessments.

Fiber and polyphenol enriched biscuits using date palm byproduct: Physiochemical characteristics, sensory properties, in vitro digestion, and storage stability.

Functional biscuit was formulated by fortifying them with polyphenolic extract and fiber-rich residue of defatted date seed powder (DDSP) obtained through microwave-assisted extraction. Effect of particle size (small, medium, and large) and substitution level (2.5%, 5%, and 7.5%) of fiber-rich residue, along with the phenolic extract, on bioactive, physical, textural, and gastrointestinal digestion of fortified biscuits was studied followed by sensory and shelf-life studies. The total phenolic content (TPC) and antioxidant properties of biscuits increased with increasing substitution levels and particle size. DDSP residue fortification increased the fiber content in biscuits. Large particles of the residue-fortified biscuits showed significantly higher (p<0.05) hardness compared to the control biscuits. Diameter of the biscuits decreased with increasing substitution level and particle size of fiber-rich residue with the lowest value of 50.66mm in 7.5% substitution of large particles. The 7.5% substitution level of small particles resulted in the lowest spread ratio of 8.97 and the highest thickness of 5.79mm. Consumer perceptions were at an acceptable level after the fortification, with an average sensory score of 6.02 out of 9 for overall acceptability. After 24 weeks storage, TPC decreased in biscuits, but TPC retention increased with increasing substitution level and particle size of residue. Thiobarbituric acid reactive substances (TBARS) value of biscuits increased with storage. The highest phenolic recovery was observed in the intestinal phase of the gastrointestinal digestion with the highest recovery of 102.33 at 2.5% level of large particles. Thus, phenolic extract and fiber-rich residue incorporation was effective to enhance the nutritional and functional properties of biscuits. PRACTICAL APPLICATION: Date seeds are rich in bioactive components and fiber. This study demonstrated the feasibility of utilizing date seeds to improve nutritional and functional properties of bakery products. The incorporation of the microwave-assisted polyphenolic extract and the fiber-rich residue of defatted date seed powder into biscuit enhanced the bioactive, nutritional, and functional characteristics while maintaining the consumer acceptance. This research contributes to the valorization of byproducts in the agriculture and food industries, promoting sustainability and a bio-circular economy.

Predicting metal-binding proteins and structures through integration of evolutionary-scale and physics-based modeling.

Metals are essential elements in all living organisms, binding to approximately 50% of proteins. They serve to stabilize proteins, catalyze reactions, regulate activities, and fulfill various physiological and pathological functions. While there have been many advancements in determining the structures of protein-metal complexes, numerous metal-binding proteins still need to be identified through computational methods and validated through experiments. To address this need, we have developed the ESMBind workflow, which combines evolutionary scale modeling (ESM) for metal-binding prediction and physics-based protein-metal modeling. Our approach utilizes the ESM-2 and ESM-IF models to predict metal-binding probability at the residue level. In addition, we have designed a metal-placement method and energy minimization technique to generate detailed 3D structures of protein-metal complexes. Our workflow outperforms other models in terms of residue and 3D-level predictions. To demonstrate its effectiveness, we applied the workflow to 142 uncharacterized fungal pathogen proteins and predicted metal-binding proteins involved in fungal infection and virulence.

The Lingering Menace: How Legacy Organochlorine Pesticides Still Threaten Our Rivers and Food Chains

The bioaccumulation of organochlorine pesticides (OCPs) in aquatic organisms has been extensively explored in recent years due to associated ecological risks and potential threats to human health through food. This study aims to assess the bioaccumulation of organochlorine pesticides (OCPs) in 18 freshwater fish species from the Pearl River Delta, China. The observed OCP concentrations ranged from 0.69 to 43.15ng/g wet weight, indicating low to moderate pollution levels. A linear mixed-effects model revealed the contribution of the feeding habits and geographic distributions at 58.67 and 0.67% of OCP accumulation, respectively. Bottom-dwelling carnivorous fish species exhibited greater OCP residue levels than those in the upper layers of the freshwater. Estuarine organisms showed higher Dichlorodiphenyltrichloroethane (DDT) residue levels than those inland species. On the other hand, although there were no direct carcinogenic or exposure risks associated with OCPs in the study area, potential related hazards were observed. Consumers are, therefore, advised to select fish species from the middle and upper delta rather than bottom fish, shellfish, and shrimp. The current research provides valuable guidance for aquatic food consumption.

Hydroxycinnamic acids mediated modulation of α-Synuclein fibrillation: Biophysical insights.

The fibrillation of α-synuclein (α-Syn) is considered a major contributor to Parkinson's disease (PD). Recent therapeutic measures have focused on inhibiting the fibrillation of α-Syn using various small molecules. We report here the effects of two different hydroxycinnamic acids; chlorogenic acid and sinapic acid on α-Syn fibrillation and have also discussed the mechanistic insights into their mode of modulation. The fluorescence spectroscopy shows that the two hydroxycinnamic acids bind with α-Syn with moderate affinity. Molecular docking studies provide a detailed insights into binding at the residue level and isothermal titration calorimetry reveals specific interactions, like hydrogen bonding, hydrophobic interactions, and van der Waals forces involved in the binding process. Fibrillation kinetics and transmission microscopic studies demonstrated that both chlorogenic acid and sinapic acid attenuate α-Syn fibrillation in a concentration dependent manner. Circular dichroism spectroscopy shows that these compounds bind with α-Syn and delay its structural transition in β-sheet containing fibrillar structures. Both the compounds are also effective even if added after the onset of fibrillation and the fibrillar species formed in the presence of these acids are unable to induce secondary nucleation in monomeric α-Syn. Such kind of structural and mechanistic insights are extremely crucial for designing therapeutic intervention in PD and other neurodegenerative diseases.

Optimized methods for the investigation of changes in levels of pesticide residues and their transformation products in iceberg lettuce

Optimized methods for the investigation of changes in levels of pesticide residues and their transformation products in iceberg lettuce

An Au-Ag@Au fiber surface plasmon resonance sensor for highly sensitive detection of fluoroquinolone residues.

Antibiotic residue detection plays an important role in protecting human health, but real-time, rapid, and highly sensitive detection is still challenging. Herein, gold and silver nanoparticles (Au-Ag NPs) were in situ grown on the surface of optical fibers and a 50 nm thick gold film was deposited on the sensor's surface to fabricate the Au-Ag@Au fiber SPR sensor. The sensitivity of the sensor reached 3512 nm per RIU in the refractive index range of 1.328-1.371. When analyzing antibiotic residues in food, the detection limits for Enro and Cip were 0.97 ng mL-1 and 0.70 ng mL-1, respectively. Their recoveries ranged from 96.64 to 115.32% and 96.18 to 121.06% in milk samples. There is a high level of antibiotic residues in meat, milk, and aquatic products and this study has significant potential in food safety testing applications. Moreover, this study will be widely used in environmental monitoring (such as heavy metal ions), medical diagnosis (viruses), marine exploration, drug screening and other analytical fields as well.

Intramolecular distance-regulated G4 DNA enzymatic activity-based chromophotometric system for visual monitoring of diquat.

As global food production continues to surge, the widespread use of herbicides has also increased concurrently, posing challenges like health risks and environmental pollution. Traditional detection methods for pesticide residues, such as diquat (DQ), were hampered by limitations like high expenses, lengthy detection times and complex operations, restricting their practical application in rapid clinical diagnosis. In light of the pressing necessity for the identification of minute pesticide residues and the intrinsic constraints of small molecule analysis, a novel chromophotometric biosensor targeting small molecules was developed based on bi-epitopes on single antibody to immobilize two DQ-PAL, inhibiting the hybridization of DQ-PAL. Accordingly, the free DQ-PAL could hybridize with each other to form a G-quadruplex for a highly selective analysis of DQ with a detection limit of 26.3pg/mL and 10pg/mL by chromophotometric and image colorimetric method respectively. Furthermore, this designed biosensor has been successfully applied to evaluate the levels of DQ residues in real samples, providing an efficient solution for the biological analysis of small molecule targets and enhancing food safety concerning pesticide residues. In comparison to conventional techniques, this biosensor has the advantages of user-friendly operations, portability, high sensitivity, low detection limit and minimal background interference, making it well-suited for clinical diagnostics. At the same time, this technology provides a new idea for the rapid in vitro detection of biological small molecules, and shows great potential applications in agricultural residue-related food safety.

Occurrence and Risk Assessment of Tetracycline Residues in Layer Eggs in Haryana, India.

Antibiotics are extensively used in layer flocks for the prevention of diseases and to enhance their growth and production. However, their nonprudent use is leading to the occurrence of residues in eggs. The present study aimed at the detection of tetracycline group residues in egg samples collected from layer farms located in Haryana, India, and human health risk assessment. A total of 100 pooled egg samples were analyzed using High-Performance Liquid Chromatography with Ultraviolet detector for the detection of tetracycline group residues. Out of 100 pooled samples, 13 (13%) were found to be contaminated with tetracycline residues (12 for chlortetracycline and one for tetracycline). Of these, five (38.5%) samples (one for tetracycline and four for chlortetracycline) exceeded the maximum residue limit (MRL) established by Food Safety and Standards Authority of India. The risk assessment based on the per capita availability of eggs in Haryana revealed that the current levels of residues in eggs pose no significant toxicological effects on the consumer's health. The residues exceeding MRL indicate nonprudent use of antibiotics in veterinary practices, which could lead to the emergence of antibiotic resistance. There is a need to generate awareness among farmers toward judicious antibiotic usage in layer birds and adherence to withdrawal periods to prevent the escalating problem of antibiotic resistance.

Simultaneous extraction and purification of polysaccharides and proteins from Pleurotus ostreatus using an aqueous two-phase system.

Pleurotus ostreatus is a nutrient-dense edible fungus renowned for its delicate texture, appealing flavor, and numerous potential health benefits. Simultaneous extraction within the framework of food resource processing facilitates the concurrent isolation and analysis of multiple target compounds. In this study, an ethanol/salt aqueous two-phase system (ATPS) was employed to extract polysaccharides (PS) and proteins from P. ostreatus. The impacts of pH, inorganic salts, and temperature on ATPS phase formation were systematically evaluated. The ethanol/K₂HPO₄ system demonstrated superior selective extraction performance under optimal conditions: 25.16% ethanol (w/w), 15.91% K₂HPO₄ (w/w), and 24.11% crude extract (w/w) without pH adjustment. The highest recovery efficiency of PS and proteins were 90.29%±0.24% and 76.35%±0.15%, respectively. The simultaneous extraction efficiency of PS and proteins was 12.49%±0.14% and 20.34%±0.09%, respectively. As a comparison, hot water extraction and alkali extraction methods were performed to assess the impact of ATPS on the physicochemical properties of PS and proteins. SDS-PAGE and HPLC analyses confirmed that the protein subunit distribution was consistent across different extraction methods, whereas the ATPS-extracted PS exhibited characteristics of homogeneous heteropolysaccharides with a molecular weight of 28.8×10⁶Da. Monosaccharides such as mannose, glucuronic acid, and glucose were identified in the PS hydrolysate. The results demonstrate that ATPS preserves the physicochemical integrity of the extracted substances. This method holds promise for unlocking new possibilities and has the potential to become an effective method for large-scale extraction and purification of polysaccharides and proteins from edible fungi. PRACTICAL APPLICATION: This work describes an efficient and straightforward aqueous two-phase system (ATPS) method for simultaneously extracting polysaccharides and proteins from Pleurotus ostreatus. This approach offers advantages such as reduced operational time, lower toxicity solvents, and minimized byproduct waste for the extraction of bioactive substances from edible fungi. Additionally, the reduced residue levels help to shorten subsequent purification steps. This promising method has potential applications in the food, pharmaceutical, and health product industries.

Multiresidue Method for Quantification of Nitroimidazoles, Anthelmintics, Amphenicols, and Dyes in Meat, Shrimp, and Fish by Using a Modified QuEChERS-type Extraction and Isotope Dilution Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry

This paper presents an analytical multiresidue method for the quantification of 7 nitroimidazoles, 19 anthelmintics, 3 amphenicols, and 4 dyes in poultry, pork, beef, horse, shrimp, and fish samples by isotope dilution ultra-high performance liquid chromatography coupled with tandem mass spectrometry (UHPLC-MS/MS) in a single 6 min run. Samples were prepared using a modified quick, easy, cheap, effective, rugged and safe (QuEChERS)-type extraction with ethyl acetate and Na2SO4-NaCl (2:1), concentration into dimethyl sulfoxide (DMSO), and defatting by liquid-liquid extraction (LLE) with n-hexane. No clean-up using solid-phase extraction (SPE) cartridges or dispersive solid-phase extraction (DSPE) was necessary. The linearity ranges (in μg kg−1) were 0.10-0.60 for chloramphenicol, 0.50-3.0 for dyes, 1.5-9.0 for nitroimidazoles, and 5.0-30.0 for the other drugs. The limits of quantitation (LOQ) were established at the lowest calibration curve levels. Except for chloramphenicol in the horse matrix, analyte recovery and reproducibility were satisfactory (recovery (fREC): 75.0 to 116.6%; coefficient of variation (CV): 1.2 to 29.9%). For the unapproved substances and the substances with a maximum residue level (MRL), respectively, the decision limits (CCα) were 0.14-4.10 and 5.28-1003.60 μg kg−1, while the detection capabilities (CCβ) were 0.13-3.33 and 5.46-11.56 μg kg−1.