Trace Analysis of Seven Neonicotinoid Insecticides in Bee Pollen by Solid–Liquid Extraction and Liquid Chromatography Coupled to Electrospray Ionization Mass Spectrometry

A new, fast, simple, and efficient sample treatment to extract seven neonicotinoid insecticides (acetamiprid, clothianidin, dinotefuran, imidacloprid, nitenpyram, thiacloprid, and thiamethoxam) in corbicular bee pollen has been developed. This procedure consisted of a solid–liquid extraction of the neonicotinoids from pollen with dichloromethane, followed by evaporation and reconstitution. Once the neonicotinoids were extracted, they were determined using a liquid chromatography coupled to an electrospray ionization mass spectrometry method. The method was validated in terms of selectivity, linearity, precision and recovery. The limits of detection and quantification were 0.4–2.8 μg/kg and 1.2–9.1 μg/kg, respectively, and the extraction recoveries were between 86 and 106 % in all cases. Finally, the proposed method was applied to analyze bee pollen samples collected from apiaries located close to fruit orchards in two Spanish regions, and traces of acetamiprid and imidacloprid were found in two samples.     

Gas chromatography-tandem mass spectrometry multi-residual analysis of contaminants in Italian honey samples

ABSTRACT

Contaminants belonging to various classes, including polychlorobiphenyls (PCBs), polycyclic aromatic hydrocarbons (PAHs), organochlorine pesticides (OCPs), organophosphorus pesticides (OPPs), pyrethroid insecticides (PYRs), fungicides (Fs), herbicides (Hs), synergists (SYNs) and insect growth regulators (IGRs) were analysed simultaneously in honey samples using a new simultaneous, easy and rapid method based on a liquid–liquid extraction with a mixture of n-hexane and ethyl acetate. It allowed recoveries in the range 80–137%, with limits of detection (LODs) between 0.10 and 5.21 ng g^–1, showing a good sensitivity and accuracy. All the analysed Italian honeys showed the presence of residues of OPPs; PAHs were in 46.8% of the samples and PCBs were always below the LODs; 53.2% of the samples were contaminated by OCPs, PYRs, SYNs and IGRs. In addition, 46.8% of the samples exceeded the maximum residue limits (MRLs) established by the European Community in honey for chlorfenvinphos (cis + trans), TPP, γ-HCH, tebuconazole, coumaphos and τ-fluvalinate (cis + trans).     

Molecularly Imprinted Polymer as Sorbent for Solid-Phase Extraction Coupling to Gas Chromatography for the Simultaneous Determination of Trichlorfon and Monocrotophos Residues in Vegetables

In this study, a molecularly imprinted polymer (MIP) was prepared using the mixture of trichlorfon and monocrotophos as the mixed template. The imprinted polymer was characterized and exhibited good recognition ability and fast adsorption–desorption dynamic toward the trichlorfon and monocrotophos. Using this imprinted polymer as sorbent, a new method of molecularly imprinted solid-phase extraction coupled to gas chromatography for the simultaneous determination of two organophosphate pesticides residues was developed. Under optimal condition, the linear range was 0.005–10.0 mg/l. At a loading flow rate of 2.0 ml/min for loading 100 ml, the detection limits were 0.28 μg/l for trichlorfon and 0.090 μg/l for monocrotophos, the peak area precision (RSD) for five replicates was 4.23–4.50 %. The blank rape samples spiked with two organophosphate pesticides at 0.05 and 0.1 mg/l levels were determined by this method with recoveries ranging from 89.41 % to 95.12 %. Moreover, this method was successfully applied to the quantitative detection of the trichlorfon and monocrotophos residues in leek samples.     

Investigation of Chlorpyrifos and Its Transformation Products in Fruits and Spices by Combining Electrochemistry and Liquid Chromatography Coupled to Tandem Mass Spectrometry

The identification of transformation products (TPs) of pesticides in food is a crucial task difficult to tackle, due to the lack of standards. In this work, we present a novel methodology to synthesize five main TP standards of the insecticide chlorpyrifos (CPF) and to investigate their occurrence in selected fruits and spices. TPs were electrochemically (EC) synthesized using a boron-doped diamond electrode (BDD) and identified by EC coupled online to mass spectrometry, LC-MS/MS, and high-resolution mass spectrometry. CPF and its TPs were analyzed in the food samples by LC-MS/MS on multiple reaction monitoring (MRM) after dispersive solid-phase extraction. A good recovery of 83–103% for CPF and 65–85% for TPs was obtained. Matrix effects, which cause signal suppression, ranged between 81 to 95% for all targeted analytes. The limit of detection and quantification for CPF were 1.6–1.9 and 4.9–5.7 μg/kg, respectively. Among investigated samples, CPF was determined in fresh lemon (104 μg/kg), fenugreek seed (40 μg/kg), and black pepper (31 μg/kg). CPF content in all samples was lower than the EU maximum residue level (MRL). The most frequently detected TPs were diethylthiophosphate and diethylphosphate. Other TPs, CPF oxon and trichloropyridinol, were also detected. Hence, EC is a versatile tool to synthesize TP standards which enables the determination of contaminants and residues in foodstuffs even if no commercial standards are available.     

Simultaneous Determination of Dimethenamid,Saflufenacil and their Metabolites in Maize Using a Modified QuEChERS Method and Liquid Chromatography-Tandem Mass Spectrometry

Hydrophilic metabolites of pesticides in food and the environment are seldom analyzed due to the lack of suitable analytical methods. In the present study, a single-run analytical method was developed to determine dimethenamid, saflufenacil and their five metabolites in maize grain and plant. A good linearity was achieved for the matrix-matched calibration curves of the seven analytes with r²?≥?0.9991. The average recoveries of dimethenamid, saflufenacil and their metabolites in maize grain and plant were 70.1–113.8% with inter-day relative standard deviations ≤?21.5%. The limits of detection and quantification for the two herbicides and their metabolites were in the ranges of 0.008–1.4 μg/kg and 0.027–4.7 μg/kg, respectively, in two matrices. The limits of quantification for dimethenamid and saflufenacil in maize grain were below the maximum residue limits proposed by Codex (10 μg/kg). The results from field trials demonstrated the method effective and reliable for monitoring of the target residues in maize.     

蜂花粉中新烟碱农药的残留分析及膳食摄入风险评估

该研究探讨了我国不同植物源66个蜂花粉样品中8种新烟碱农药的残留情况,并根据残留结果进行普通人群膳食摄入风险评估。结果发现,样品检出率为50.0%,共检出5种新烟碱农药,包括啶虫脒、吡虫啉、噻虫嗪、噻虫胺和呋虫胺,检出率最高的为噻虫嗪（31.8%）,残留浓度最高为啶虫脒（195.1 ng/g）。4种植物源的蜂花粉中新烟碱农药的残留存在显著差异：茶花粉的检出率显著高于其他3种花粉;杂花粉的残留浓度显著高于茶花粉和油菜花粉,残留浓度从高到低依次为杂花粉、荞麦粉、茶花粉、油菜花粉。来自6个主要地区的蜂花粉残留情况也有所不同,这可能跟我国不同地区和不同作物中新烟碱农药的施用情况相关。依据新烟碱农药的残留浓度进行人类膳食摄入风险评估,评估结果（风险商值均小于1%）说明蜂花粉中的新烟碱农药残留风险可接受。     

Rapid Determination of Organonitrogen, Organophosphorus and Carbamate Pesticides in Tea by Ultrahigh-Performance Liquid Chromatography–Tandem Mass Spectrometry (UPLC-MS/MS)

A rapid and effective multiresidue method has been developed for the determination of 18 pesticide residues (selected from organonitrogen, organophosphorus, and carbamate pesticides) in tea by ultrahigh-performance liquid chromatography–tandem mass spectrometry. Tea samples were extracted with acetonitrile and purified by a novel multilayer solid-phase extraction cartridge—Cleanet TPT. Evaluation of the influence of the mobile phase on the ionization efficiency, resolution, and sensitivity was carried out by comparing the acetonitrile–water and methanol–water with different modifiers. The recoveries of all the pesticides varied from 70 to 110 % with a relative standard deviation of less than 15 %, and the determination coefficient for each pesticide was R ²?>?0.99. Matrix-matched standard calibration curve was used to reduce errors associated with matrix-induced enhancement or suppression effects. The limit of detection for all targeted pesticides ranged from 0.03 to 1.5 μg/kg. Applicability of this analytical approach was confirmed by successful determination of tea samples from different regions of China.     

Method Development,Optimization and Validation of Matrix Hydration Effect on Pesticide Residues in Cocoa Beans Using Modified QuEChERS Method and Gas Chromatography Tandem Mass Spectrometry

Modified QuEChERS method combined with gas chromatography tandem mass spectrometry (GC-MS/MS) was developed and validated to determine pesticide residues in dried cocoa beans. Extraction efficiency of matrix hydration effect on 19 pesticide residues was studied and optimized using 2³ full factorial design with percentage recoveries as the response variable. The optimized hydration method was validated for 24 pesticides, and recoveries obtained were in the range of 70–120% with relative standard deviations of less than 20% for most pesticides. Limit of quantification was obtained at 10 μg/kg for all pesticides, and this value was lower than national maximum residue levels (MRLs). Finally, the developed and optimized method was applied to real cocoa bean samples and the results from incurred residues were compared between method with and without matrix hydration. These results suggest that the addition of water to the dry and high-fat cocoa bean samples is crucial in pesticide residue analysis.     

Survey of organophosphorus pesticide residues in virgin olive oils produced in Chile

Dimethoate, diazinon, parathion methyl, pirimiphos methyl, malathion, fenthion, chlorpyriphos, methidathion and azinphos methyl were determined in 71 olive oil samples produced in Chile from different varieties of olives (arbequina, frantoio, picual, lechino and blend) at three different harvest periods (2007, 2008 and 2009). The target pesticides were determined using a validated analytical method based on microwave-assisted liquid–liquid and solid-phase extraction with subsequent GC–FPD detection and GC–MS/MS for confirmation purposes. In 79% of the samples, five of the nine pesticides tested were detected with a frequency of one pesticide per sample. The highest detection rates were observed for the residues of chlorpyriphos and diazinon. The average concentration of chlorpyriphos, diazinon, azinphos methyl and methidathion were 0.084, 0.057, 0.024 and 0.010 µg g^?1, respectively. Higher contents of organophosphorus pesticides (OPPs) were found in regions where intensive agriculture is practiced. However, the levels of OPPs were reassuringly low and indicate that olive oil produced and exported from Chile does not currently represent any risk for consumers.     

Multi-residual Pesticide Monitoring in Commercial Chinese Herbal Medicines by Gas Chromatography–Triple Quadrupole Tandem Mass Spectrometry

To investigate multi-residual pesticide monitoring data in commercial Chinese herbal medicines on major markets, an easy, rapid, and selective gas chromatography with mass spectrometry (GC/MS/MS) method was established for simultaneously determining multi-residual pesticides including organochlorine, pyrethroid, carbamate, and organophosphorus pesticides in Chinese herbal medicines. The analytical method was based on an efficient extraction procedure and further cleanup steps by solid-phase extraction columns, yielding recovery rates in the range of 70.0–120.0 % for the majority of pesticides, except for hexachlorobenze, diazinon, β-HCH, δ-HCH, and omethoate, with precision values expressed as relative standard deviation of 0.1–14.7 %. The limits of detection of the established GC/MS/MS method for all investigated pesticides ranged from 0.01 to 3.6 μg kg^?1 and limits of quantification from 0.03 to 11.88 μg kg^?1. With this validated method, multi-residual pesticides of 132 Chinese herbal medicine samples were analyzed. The monitoring results indicated that pesticide residue was found in 74 samples. In total, 51 pesticides were found with detection rate ranging from 0.76 to 18.94 %. An 82.3 % of positive pesticides were found in less than 6 % of samples. Hexachlorobenzene was found in 25 samples, quintozene in 15 samples, and acephate and simazine in 13 samples. Concentrations of pesticide residue from monitoring data obtained ranged from 0.5 to 203.5 μg kg^?1. The simple and rapid method can be used as routine analysis method in multi-residual pesticide monitoring of Chinese herbal medicines.     

Dietary exposure of Hong Kong adults to pesticide residues: results of the first Hong Kong total diet study

The use of pesticides and other chemicals has become a common practice in modern agriculture to enhance and stabilise crop yield, protect the nutritional integrity of food, facilitate food storage to assure year-round supplies, and provide attractive and appealing food products. With the adoption of strict good agricultural practice (GAP), only minimal amounts of pesticide residues should remain on the crops or in connected foods of animal origin up the food chain. To assess their associated health risk to local people, the dietary exposure of Hong Kong adults to residues of four groups of pesticides or their metabolites – organophosphorus pesticides (OPPs), carbamates, pyrethrins and pyrethroids, and dithiocarbamate (DTC) metabolites – is estimated in the first Hong Kong Total Diet Study (TDS). A total of 150 commonly consumed food items were collected and prepared “as consumed”. A total of 600 composite food samples were analysed for 85 pesticides or their metabolites by liquid chromatography-tandem mass spectrometry (LC-MS/MS). These pesticides were primarily found at low levels (highest mean = 350 μg kg^?1) in food samples of plant origin such as vegetables and fruits. Dietary exposures to pesticide residues were estimated based on the analytical results and the food consumption data of the local residents. The estimated dietary exposures of Hong Kong adults to all individual pesticides were well below their respective acceptable daily intakes (ADIs). The percentage contributions of the estimated mean and 95th percentile dietary exposures to the ADIs of individual pesticides were <6% and <24% for the OPPs, <1% for the carbamates and pyrethrins and pyrethroids, and <1% and <4% for the DTC metabolites, respectively. The findings indicate that dietary exposures to all the pesticide residues analysed in this study were unlikely to pose unacceptable health risks to the Hong Kong population.     

Investigation of Levels and Fate of Pyridalyl in Fruit and Vegetable Samples by Fast Gas Chromatography–Mass Spectrometry

The search on pyridalyl residues, the novel insecticide, in strawberries and spring onions was evaluated. The QuEChERS technique was used for sample preparation. A fast gas chromatography–mass spectrometry (GC–MS) method was developed and validated for the analysis of pyridalyl in both matrices. Fast GC–MS was performed with a narrow-bore capillary column and a quadrupole mass detector with electron ionization and negative chemical ionization, both operating in selected ion monitoring mode. Fortification studies at 1, 5, 10, and 250 μg/kg for fruit and vegetable matrices were performed. Recoveries for all fortification levels, two ionization modes ranged from 72 to 114 %. Matrix effects were discussed. Limits of quantification were established at 1 μg/kg. Field experiments to investigate the pre-harvest interval were carried out. The proposed method was applied successfully to the determination of pyridalyl residues in samples available on Slovak market, and none of the samples contained detectable amounts of pesticides. The developed method is simple, efficient, and easy to adopt in laboratories engaged in pesticide residue analysis method.     

Determination of Some Endocrine-Disrupting Metals and Organochlorinated Pesticide Residues in Baby Food and Infant Formula in Turkish Markets

There is a paucity of data in respect of the nutritional quality of complementary foods for infants and young children aged between 6 and 12 months. In this study, we developed and validated an analytical method for determination of the endocrine-disrupting organochlorine pesticides (OCPs) and elements (As, Cd, and Pb) in infant formula and baby foods. Therefore, it found out the contamination level of the both OCPs and some trace metals (As, Cd, and Pb) in widely consumed infant formula and baby food in Turkey. Metal concentrations in baby foods and infant formula were determined by inductively coupled plasma mass spectrometry. Samples were digested with nitric acid and hydrogen peroxide in a microwave oven. Determination of 24 organochlorine pesticide residues in baby foods and infant formula was completed by using gas chromatography double mass spectrometry. QuEChERS extraction method was carried out in the sample preparation part. The analytical performance of the entire procedure, such as linearity, the detection of limit, limit of quantification, specificity/selectivity, recovery (%), and precision, were assessed. The recoveries ranged from 93% (As) to 100% (Pb) for elements 78–98% for organochlorine pesticide residues (OCPs) at 100 ng mL^?1. According to the results, lead, cadmium, and pesticides were not detected in any of the samples, while arsenic was detected in 16 samples.     

Fast Preconcentration of Pesticide Residues in Oilseeds by Combination of QuEChERS with Dispersive Liquid–Liquid Microextraction Followed by Gas Chromatography-Mass Spectrometry

A fast, efficient, and simple method for determination of pesticide residues in pumpkin seeds has been developed combining QuEChERS and dispersive liquid–liquid microextraction (DLLME) followed by gas chromatography and mass spectrometry (GC-MS). Parameters affecting the DLLME performance such as solvent selection and volume of extractive and dispersive solvent, salt effect, and extraction time were studied. Under the selected conditions (50 μL extractive solvent chloroform, 1 mL QuEChERS extract, and 3 mL water), the developed method was validated. Linearity was evaluated at nine concentrations in the broad range of 0.1–500 μg/kg with correlation coefficients from 0.9842 to 0.9972. The relative standard deviations at lowest calibration level varied from 0.3 to 22 %. Under the optimum conditions, an enrichment factor was 6–17-fold and detection limits 0.01–12.17 μg/kg were achieved. Finally, the developed and validated method was successfully applied for the extraction and determination of pesticide residues in 16 real samples with 2 positive findings below maximum residue limits (MRL). Limits of detection (LODs) of the proposed method are below the MRLs established by the European Union.     

Determining pesticide residues in wheat flour by ultrahigh-performance liquid chromatography/quadrupole time-of-flight mass spectrometry with QuEChERS extraction

ABSTRACT

Pesticides are used to increase crop yields and preserve quality by protecting crops against pests; however, their overuse can adversely affect human health and the environment. Herein, we report the development of a multi-pesticide screening method using optimized QuEChERS coupled with liquid chromatography/quadrupole time-of-flight (QTOF) mass spectrometry for the analysis of 13 pesticides in wheat flour. Mass accuracies with errors of less than 2.4 ppm were obtained for all analysed pesticides, and the method provided satisfactory recovery and linearity. Repeatabilities of 0.3–12.7% and reproducibilities of 2.5–15.2% were observed in full-scan TOF mode. The performance of the developed full-scan TOF method was compared to that obtained in high-resolution multiple reaction monitoring (MRM-HR) mode. The limits of quantification for the full-scan TOF and MRM-HR modes ranged from 2 to 10, and 3 to 9 μg kg^?1, respectively. The two quantification methods exhibited high sensitivities (limit of detections: 1–3 μg kg^?1 in full-scan TOF, and 1–3 μg kg^?1 for MRM-HR mode). No pesticide residues were detected when the developed method was applied to 22 real wheat flour samples.     

Sample preparation method for the analysis of some organophosphorus pesticides residues in tomato by ultrasound-assisted solvent extraction followed by dispersive liquid–liquid microextraction

A very simple and economic method for organophosphorus pesticides (OPPs) residues analysis in tomato by means of gas chromatography–flame photometric detection (GC–FPD) has been developed. The method involves a rapid and small-scale extraction. The sample was homogenised and extraction of the OPPs with acetone was carried out assisted by sonication. No clean-up or evaporation were required after extraction. Pre-concentration of the OPPs from the acetone extract was done by using dispersive liquid–liquid microextraction (DLLME) technique. Chlorobenzene was added in micro-level volume as extraction solvent and triphenylphosphate as internal standard in DLLME procedure. The method showed good linearity over the range assayed (0.5–1000 μg kg⁻¹) and the detection limits for the pesticides studied varied from 0.1 to 0.5 μg kg⁻¹. Repeatability studies resulted a relative standard deviation lower than 10% in all cases. The proposed method was used to determine pesticides levels in tomatoes grown in open field.     

Direct Competitive Biomimetic Immunoassay Based on Quantum Dot Label for Simultaneous Determination of Two Pesticide Residues in Fruit and Vegetable Samples

In this study, trichlorfon and chlorpyrifos conjugated to CdSe/ZnS quantum dots with different emission wavelengths were adopted as labels. A hydrophilic imprinted film synthesized directly on the surface of a 96-well plate was used as the antibody. A direct competitive biomimetic immunoassay method for simultaneous determination of trichlorfon and chlorpyrifos in fruits and vegetables was developed. Under optimal conditions, the limit of detection of this method was 18.0 μg/L for chlorpyrifos (55 mg/kg for sample) and 19.0 μg/L for trichlorfon (45 mg/kg for sample). Orange and carrot samples spiked with chlorpyrifos and trichlorfon were extracted and determined by this method with recoveries ranging from 77.8 to 92.0%. The method was applied for detection of chlorpyrifos and trichlorfon residues in banana and apple samples, and the results correlated well with those obtained using gas chromatography.     

Multiresidue Analysis of 113 Pesticides in Different Maturity Levels of Mangoes Using an Optimized QuEChERS Method with GC-MS/MS and UHPLC-MS/MS

In this study, a simple and high-throughput multiresidue pesticide analysis method based on the quick, easy, cheap, effective, rugged, safe (QuEChERS) extraction combined with gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS) and ultra-high performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS) is presented for the determination of 113 pesticides in green and ripe mangoes. Different buffer systems and purification sorbents were optimized to get better recovery. Extracts from mangoes after acid acetonitrile and ammonium acetate extraction were directly injected to UHPLC-MS/MS analysis, whereas other GC-amenable compounds were treated with cleanup approaches with a mixture of sorbents [400 mg primary-secondary amine (PSA) and 400 mg graphitized carbon black (GCB)] for GC-MS/MS analysis. Recoveries for the majority of pesticides at spike levels of 10, 50, and 100 μg/kg were ranged between 70 and 120% with RSD values below 20%. Limits of detection (LODs) were below 4 μg/kg, whereas limits of quantification (LOQs) were below 10 μg/kg. Response linearity was good in the range between 5 and 500 μg/kg. The matrix effect for 56 pesticides by GC-MS/MS analysis exhibited a non-significant matrix effect (≤?25%) in green and ripe mangoes. For 57 pesticides used for UHPLC-MS/MS analysis, the optimized method in green mango provided no significant matrix effect (≤?25%) for 63% of the compounds, whereas only for 16 and 21% compounds, the matrix effect was medium (25–40%) and strong (>?40%); the optimized method in ripe mango provided no significant matrix effect (≤?25%) for 61% of the compounds, whereas only for 26 and 12% compounds, the matrix effect was medium (25–40%) and strong (>?40%). Following the application of a “top-down” approach, the expanded measurement uncertainty was both 21% on average (coverage factor k =?2, confidence level 95%) in green and ripe mangoes. The application of GC-MS/MS and UHPLC-MS/MS coupled with the modified QuEChERS extraction procedures was proved to adequately quantitate these pesticides in different maturity levels of mangoes.     

凝胶渗透色谱净化系统与气相色谱-串联质谱法检测5种食品中14种有机磷和7种拟除虫菊酯类农药残留

建立GPC与GC-MS/MS测定5种食品中14种有机磷和7种拟除虫菊酯类农药残留的方法,初步分析GPC净化技术及MS/MS分析技术在食品农药多残留分析的优势。方法 用GPC作为样品前处理方法,处理韭菜、大白菜、辣椒、猪肉、鱼肉五种食品,用 GC-MS/MS检测并进行定性、定量分析。结果 GPC与GC-MS-MS检测食品中14种有机磷和7种拟除虫菊酯类农药方法的线性相关系数r＞0.995,定量限为0.002～0.034 mg/kg,对韭菜、猪肉样品按0.05、0.10、0.20 mg/kg三组水平加标测试,方法精密度RSD%为2.9～10.2%,回收率为78.6～108.3%。结论 本方法检测样品范围广、灵敏度高、定性可靠、定量准确,适合多种类食品中农药多残留分析。     

Determination of 103 Pesticides and Their Main Metabolites in Animal Origin Food by QuEChERS and Liquid Chromatography–Tandem Mass Spectrometry

A rapid and sensitive analytical multiresidue method has been developed for the simultaneous determination of 103 pesticides (herbicides, insecticides, and fungicides) and 18 metabolites in foods of animal origin using liquid chromatography-tandem with triple quadrupole in dynamic multiple reaction monitoring (DMRM) mode. A modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) sample preparation technique was established, and the efficiency of the dispersive solid-phase extraction (d-SPE) cleanup step was evaluated by comparing the effects of different d-SPE sorbent combinations (primary secondary amine (PSA) + graphitized carbon black (GCB), PSA + C18, C18, and C18 + GCB). The limits of quantification (LOQs) ranged from 1 to 10 μg/kg, and the coefficient of determination (R ²) was ≥0.995 within the calibration linearity range of 0–250 μg/L for all pesticides. The combination of C18 + GCB was validated at two spiking levels (10 and 50 μg/kg) in chicken, fish, pork, and rabbit. Satisfactory recoveries (70–119%) and RSDs ≤17% were achieved for all analytes, except for naptalam (60–69%), pyrimethanil (40–49%), and thiabendazole (62–66%) at 10 μg/kg spiking level. The validated method was successfully applied to the analysis of real samples of food of animal origin.