The use of pesticides and veterinary drugs results in the appearance of residues of xenobiotics in foods. Thus, several methods have been developed for monitoring them; however, most are tedious and expensive. By contrast, the QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) methodology involves a microextraction that yields small samples and has been applied for the analysis of various xenobiotics including pesticides, antibiotics, and mycotoxins. QuEChERS has shown advantages over other techniques including fast sample preparation, reduced needs for reagents and labware, and versatility. This approach allows the simultaneous determination of pesticides with various polarities and volatilities and can be easily modified for the analysis of a wide range of xenobiotics in various matrices including animal products rich in fat. Nevertheless, to attain high recoveries, the extraction, cleanup, and concentration steps have to be optimized according to the target compounds and matrix. Hence, QuEChERS is a promising and environmentally friendly methodology for the high-throughput routine analysis of xenobiotics in animal products. This review focuses on the application of QuEChERS to foods of animal origin and describes recent developments for the optimization of the analysis of veterinary drugs, pesticides, polycyclic aromatic hydrocarbons, and other compounds of concern.
The QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) methodology was reported for the first time in 2003 by Anastassiades and coworkers as an alternative to traditional pesticide analysis [
Flowchart of the QuEChERS method (based on [
Comparison of the recoveries obtained using QuEChERS with those obtained with other extraction methods (OPP: organophosphate pesticides, SPE: solid-phase extraction, SPME: solid-phase microextraction) for selected classes of compounds according to published data [
QuEChERS was originally developed as a multiclass residue method for determining pesticides in fruits and vegetables [
Because pesticides are not the only xenobiotics in foodstuffs, analysis of veterinary drugs, mycotoxins, and other contaminants cannot be neglected. So far, QuEChERS has been predominantly applied for the analysis of contaminants in foods of plant origin. In addition to pesticides in various fruits and vegetables [
QuEChERS has been demonstrated to be an effective and versatile technique and has also been recently applied for the analysis of various xenobiotics in animal products. The complexity of animal tissues and milk as well as the presence of fat are challenges to overcome for the successful analysis of xenobiotics in such matrices. Although several matrix-specific methods are reported here, it is noteworthy that a simple, modular QuEChERS method was developed for analyzing pesticides in animal products with various contents of fat, attaining adequate recoveries that could make it a good option for routine sample screening; this method involved extraction of the sample in acetonitrile, followed by hexane extraction in the presence of a QuEChERS salt and cleanup by SPE (C18) [
Therefore, this review presents a compilation of examples of the application of QuEChERS to the analysis of xenobiotics including pesticides, mycotoxins, and veterinary drugs in animal products such as meat, milk, eggs, and honey (Table
Summary of applications of QuEChERS for the analysis of xenobiotics in animal products.
Matrix | Analytes | QuEChERS method | Analytical method | Ref. |
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Goat’s milk and sheep muscle | Monepantel and its sulfone metabolite | Milk (10 g) was extracted with MeCN (12 mL) in the presence of MgSO4 and NaCl, followed by d-SPE using MgSO4 and C18. Homogenized meat (10 g) was extracted with MeCN (10 mL); MgSO4 and NaCl were added, and the supernatant was cleaned up with MgSO4 and C18. Extracts were concentrated before analysis. | UPLC-MS/MS | [ |
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Beef muscle | Cephalosporins | Homogenized beef (4 g) was extracted with 15 mL of MeCN/water (80 : 20); d-SPE was performed using C18, PSA and MgSO4. The sample was dried and reconstituted before analysis. | LC-MS/MS | [ |
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Meat and bovine fat | Chlorfenvinphos, fipronil, and cypermethrin | For the meat, 2 g of homogenized sample was extracted in 4 mL of MeCN in the presence of MgSO4 and NaCl, followed by d-SPE with C18, PSA, and MgSO4. For the fat, 1 g of homogenized sample was extracted in 5 mL of hexane + 10 mL of water + 10 mL of MeCN in the presence of MgSO4 and NaCl, followed by d-SPE with PSA and MgSO4. | GC-MS | [ |
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Bacon | Nitrites | Comminuted cooked bacon (5 g) was extracted with 10 mL of MeCN/water (1 : 1) in the presence of HCO2NH4, followed by d-SPE using MgSO4, PSA, C18, and Z-Sep sorbents. Coextracted lipids were removed by hexane partitioning. | GC-MS/MS | [ |
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Meat products | Polychlorinated biphenyls (PCBs) | Melted fat sample (1 g) was extracted with 7 mL of acetone. The supernatant was dried and collected using 2 mL of acetonitrile in the presence of PSA and MgSO4. The sample was dried and collected using isooctane before injection. | GC-MS | [ |
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Sheep meat | Chlorinated hydrocarbon and synthetic pyrethroids | Homogenized meat (10 g) was extracted with 20 mL of MeCN in the presence of MgSO4 and NaCl, followed by d-SPE using PSA and MgSO4. Samples were dried and redissolved before analysis. | GC-ECD | [ |
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Pork | Ractopamine | Ground pork sample (5 g) was extracted with 10 mL of 0.1% AcOH in MeCN, followed by cleanup using MgSO4, NaCl, C18, and PSA. Samples were dried and redissolved before analysis. | LC-MS | [ |
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Pork | Methenamine | Homogenized sample (2 g) was extracted with 10 mL of MeCN in the presence of Na2SO4, followed by extraction with MeCN-saturated hexane. The MeCN was cleaned up with PSA. | LC-MS/MS | [ |
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Chicken | Amantadine and rimantadine | Homogenized chicken meat (3 g) was extracted with 10 mL of 1% AcOH in MeCN in the presence of NaCl and MgSO4, followed by d-SPE using C18. The sample was dried and redissolved before analysis. | UHPLC-LTQ Orbitrap MS | [ |
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Chicken | Antiviral drugs and relevant metabolites | Homogenized chicken meat (2 g) was extracted with 9 mL of 1% AcOH in MeCN + 1 mL of water. The supernatant was split into two portions for the analysis of different compounds and dried. One portion was redissolved in MeOH/water and the other in water. The extracts were cleaned up using PSA. | UPLC-MS/MS | [ |
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Chicken | Veterinary drugs | Homogenized chicken meat (5 g) was extracted with 10 mL of 1% AcOH in MeCN: water (80 : 20) in the presence of Na2HCit·1.5H2O, Na3Cit·2H2O, and MgSO4, followed by d-SPE using PSA. | UHPLC-MS/MS | [ |
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Chicken | Sulfonamides | Homogenized chicken meat (10 g) was extracted with 15 mL of 1% AcOH in MeCN in the presence of NaOAc and MgSO4, followed by d-SPE using PSA and MgSO4. The sample was concentrated before analysis | HPLC-DAD | [ |
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Milk and honey | Chloramphenicol, thiamphenicol, and florfenicol | Sample (2 g) was extracted with 15 mL of 0.1% AcOH in MeCN in the presence of Na2SO4 and NaCl, followed by d-SPE using Na2SO4, C18, and QuE Z-Sep+. Samples were dried and reconstituted before analysis. | LC-MS/MS | [ |
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Milk | Anabolic steroids and agonists | Milk (5 g) was extracted with 10 mL of 5% AcOH in MeCN in the presence of ZnO nanoparticles, followed by d-SPE using PSA. Samples were dried and redissolved before analysis. | UHPLC-MS/MS | [ |
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Yogurt and milk | Herbicides (triazines and phenylureas) | Sample (5 mL) was adjusted to pH 7 and extracted with 8 mL EtOAc/hexane (1 : 1) in the presence of NaCl, followed by d-SPE using PSA. The extract was dried and redissolved before analysis. | HPLC-DAD | [ |
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Milk | Pesticides | Milk (15 g) was extracted with 15 mL of 0.1% AcOH in MeCN in the presence of NaOAc and MgSO4, followed by d-SPE using MgSO4, PSA and C18. | GC-ECD and GC-MS | [ |
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Milk | Pesticides | Milk (20 mL) was extracted with 16 mL MeCN in the presence of NaCl and MgSO4. The extract was dried and reconstituted, followed by d-SPE using PSA, Z-Sep, and Z-Sep Plus. The supernatant was dried and redissolved before analysis. | HPLC-DAD | [ |
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Raw milk (cow, goat, and buffalo milk) | Steroid hormones | Milk (10 g) was extracted with 10 mL MeCN in the presence of NaCl, Na2HCit, Na2HCit·1.5H2O, and MgSO4, followed by d-SPE using MgSO4, PSA, and acidic alumina. | UPLC-QTOF-MS | [ |
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Milk | Sulfonamides | Milk (10 g) was extracted with 10 mL of 1% AcOH in MeCN + 10 mL 0.1 M EDTA in the presence of NaOAc and MgSO4. | LC/MS/MS | [ |
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Eggs | Aflatoxins B1, G1, B2, G2, zearalenone, and its metabolites | Homogenized eggs (2 g) + 2 mL water was extracted with 10 mL of 1% AcOH in MeCN in the presence of MgSO4 and NaCl, followed by d-SPE using MgSO4 and C18. The extract was dried and redissolved before analysis. | UPLC-MS/MS | [ |
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Eggs | Melamine and cyromazine | Homogenized egg yolk (0.5 g) was extracted with 1 mL MeCN + 1 mL MeOH in the presence of QuEChERS sorbent for fatty samples. The extract was dried and redissolved before analysis. | HPLC-DAD | [ |
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Eggs | Melamine and cyromazine | Homogenized egg sample (1 g) was extracted with 5 mL MeCN + 0.1 M HCl (99.5 : 0.5), followed by d-SPE using MgSO4 and GCB. The extract was dried and redissolved before analysis. | LC-MS/MS | [ |
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Eggs | Mycotoxins | Homogenized egg (2 g) was extracted with 10 mL of MeOH/water (80 : 20) with 1% AcOH, Na2SO4, and NaOAc, without d-SPE. | UHPLC-MS/MS | [ |
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Eggs and egg products | Pesticides | Homogenized egg (5 g) was extracted with 1% AcOH in MeCN (15 mL) in the presence of MgSO4 and NaOAc, followed by d-SPE with MgSO4, C18, PSA, and GCB. The extract was dried and redissolved before analysis. | LC-MS/MS | [ |
In the case of egg yolk, 2.5 g of homogenized sample + 2.5 mL of deionized water were mixed prior to extraction, performed as above. Powdered egg white was diluted to 12.3% w/v with deionized water, and a 5 g sample was extracted as above. | ||||
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Eggs, chicken, and pork | Phorate and its metabolites | Homogenized sample (5 g) was extracted with 15 mL of 1% AcOH in MeCN in the presence of MgSO4 and NaOAc; the supernatant was reextracted with 1% AcOH in MeCN, cleaned up with MgSO4, PSA, and C18. The extract was dried and redissolved before analysis. | UHPLC-MS/MS | [ |
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Fish (tilapia and salmon) | Organochlorine pesticides and polychlorinated biphenyls | Homogenized fish (5 g) was extracted with 10 mL of Milli-Q water + 10 mL of MeCN in the presence of MgSO4, NaCl, Na2HCit·1.5H2O, and Na3Cit·2H2O. The supernatant was frozen and partitioned in CaCl2, followed by a second cleanup with MgSO4 and PSA. | GC-MS | [ |
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Fish | Organochlorine pesticides | Homogenized fish (5 g) was extracted with MeCN (10 mL) in the presence of MgSO4 and NaCl, followed by d-SPE using PSA. Then, water and 1-undecanol were added, and the sample was cooled in an ice bath to separate the organic phase. | GC-MS | [ |
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High-fat smoked salmon | Parent and substituted polycyclic aromatic hydrocarbons | Four QuEChERS extraction methods were tested. Optimized QuEChERS involved extraction with 2 : 2 : 1 (v/v/v) acetone/ethyl acetate/isooctane in the presence of AOAC or EN salts, followed by d-SPE with Sampli-Q AOAC fatty sample d-SPE tubes. | GC-MS | [ |
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Fish muscle and liver tissues | Personal care products (biocides, synthetic musks, and benzotriazoles) | Homogenized fish muscle (2 g) or fish liver (0.5 g) was extracted with 1% AcOH in MeCN (10 mL) in the presence of MgSO4 and NaOAc, followed by d-SPE using PSA, MgSO4, and C18. The sample was evaporated and redissolved before analysis. | UPLC-MS/MS and GC-MS | [ |
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Fish (carp and sturgeon) | Organochlorine and organophosphate pesticides | Homogenized fish muscle (5 g) was extracted with MeCN (10 mL) in the presence of Na2HCit·1.5H2O, Na3Cit·2H2O, NaCl, and MgSO4. A dual d-SPE cleanup was performed, using PSA + SAX + NH2, followed by C18 and CHCl3 addition and freezing-out to remove fats. | GC/Q-MS | [ |
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Fish (catfish) | PCBs | Homogenized sample (3 g) was extracted with water (5 mL) and MeCN (30 mL) in the presence of MgSO4 and NaCl; d-SPE was performed with MgSO4, PSA, and C18. | GC-MS | [ |
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Fish | Quinolones | Homogenized fish (5 g) was extracted with 5% HCOOH in MeCN (10 mL) in the presence of MgSO4, NaCl, NaOAc, and Na2HCit·1.5H2O, followed by d-SPE using C18 and MgSO4. The extract was dried and redissolved before analysis. | UHPLC-FLD | [ |
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Fish | Organochlorine pesticides | Homogenized fish (5 g) was extracted with MeCN (5 mL) in the presence of MgSO4 and NaCl, followed by d-SPE with PSA + DLLME-SFO with 1-undecanol + water, and the sample was cooled in an ice bath to separate the organic phase. | GC-ECD | [ |
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Bivalves | Pharmaceuticals | Frozen-dried sample (1 g) was mixed with 10 mL water and extracted with MeCN (10 mL) in the presence of EN salts, followed by cleanup with silica gel. The extract was dried and redissolved before analysis. | LC-MS/MS | [ |
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Bivalves | Paralytic shellfish poisoning toxins | Homogenized sample (1 g) was extracted twice with 1% HCOOH (1 mL); protein was precipitated and d-SPE was performed using ABS Elut-NEXUS phase. | LC-MS | [ |
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Honey | Nitrofuran metabolites and nitroimidazole | Honey (1 g) was extracted using 10 mL MeCN with MgSO4 and NaCl, without d-SPE. The extract was evaporated and redissolved before analysis. | LC-MS/MS | [ |
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Honey | Pesticides | Honey (2.5 g) was heated in a water bath and extracted with 5 mL Na2EDTA + 5.0 mL MeCN in the presence of MgSO4 and NaCl, followed by d-SPE using PSA and MgSO4. | GC-ECD | [ |
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Honey | Pesticides | Honey (5 g) dissolved in 10 mL water was extracted with 10 mL 1% AcOH in MeCN:EtOAc (70 : 30), in the presence of MgSO4 and NaOAc, followed by d-SPE using MgSO4, Florisil, and PSA. | UHPLC-MS/MS | [ |
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Honey | Pesticides, PAHs, and PCBs | Honey (5 g) dissolved in 10 mL water was extracted with 10 mL MeCN in the presence of citrate salts, followed by d-SPE using PSA. Extracts were evaporated and redissolved; one part was directly analyzed by LC, whereas the other part was diluted with salted water and extracted with SPME for GC analysis. | LC-MS/MS, GC-MS/MS | [ |
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Honey | Pyrrolizidine and tropane alkaloids | Homogenized honey (1.5 g) was dissolved with 0.1 M H2SO4 (10 mL), and Zn dust was added. After centrifugation, the sample was extracted with 10 mL MeCN in the presence of EN salts, followed by d-SPE with Q-Sep sorbent. The extract was dried and redissolved before analysis. | LC-HRMS | [ |
Veterinary drug residues are xenobiotics of concern in meat products. These drugs include antibiotics, antiparasitic agents, compounds that stimulate muscle production, growth hormones, and anti-inflammatories. Residues of pesticides and tranquilizers can also be found in meat, and dangerous compounds like nitrosamines can be present in processed meat products. Therefore, monitoring of these substances in meat is crucial.
The first report of QuEChERS applied to animal tissues described the analysis of β-lactam antibiotics in bovine kidneys [
Antiparasitic drugs are administered to farm animals to control roundworm infections. Some common anthelmintic drugs include benzimidazoles, macrocyclic lactones, and amino-acetonitrile derivatives. As with antibiotics, residues of these compounds can show up in meat and milk and should thus be monitored. Kinsella et al. [
QuEChERS can also be used to detect the presence of residues of banned feed additives that could appear in animal products. Ractopamine is a β-agonist used as a feed additive for finishing pigs as it promotes the production of muscle instead of fat. Nevertheless, β-agonists may produce toxic effects on the cardiovascular system [
As previously mentioned, the QuEChERS methodology was originally developed for the analysis of pesticide residues in vegetables and fruits and has been successfully applied for determining pesticides in various foodstuffs. Examples of QuEChERS application for determining pesticide residues in meat include the analysis of organochlorine pesticides and pyrethroids in sheep meat [
In addition to organochlorine pesticides, polychlorinated biphenyls (PCBs) are other type of persistent organic pollutants that may contaminate meat. Even though PCBs were banned decades ago, their residues still appear in food products because of their stability and lipid-soluble properties; these compounds have harmful effects on human health including carcinogenicity, neurotoxicity, and developmental disorders in children. A QuEChERS-GC-MS method for determining PCBs in meat was optimized and successfully applied for analyzing processed meat products [
Some harmful compounds are formed during meat processing or cooking. This is the case of nitrosamines, carcinogens produced when cooking cured meats. The US Department of Agriculture Food Service and Inspection Service (USDA-FSIS) has established a method for determining nitrosamines using supercritical fluid extraction followed by GC-thermal energy analysis (GC-TEA) [
As with cattle, veterinary drugs are administered to chicken and other birds raised for food to fight infections and promote growth. Thus, residues of these substances must be monitored to ensure the safety of the meat and avoid potential harmful effects among consumers.
Sulfonamides, also known as sulfa drugs, are synthetic antibiotics used to combat bacterial infections. Nevertheless, allergic reactions to these drugs are common, and residues should be monitored to ensure they are not present at levels above those considered safe. A QuEChERS-HPLC-DAD method for detecting sulfonamides in chicken breast was reported in 2013; the method attained LOQs below the MRL established by the European Community (100 µg/kg) and recoveries above 70% [
Effects of (a) using the original or buffered QuEChERS and (b) concentrating the extract on the recovery of sulfonamides (sulfadiazine (SDZ), sulfamethoxypyridazine (SPZ), and sulfamethoxazole (SMX)) from chicken. Taken from [
Bird influenza is a serious problem that not only causes economic losses but also puts human health at risk. In the past, antiviral drugs were administered to chickens to protect them against influenza; however, the risk of resistance development by the influenza viruses, which would render drugs like Tamiflu ineffective, motivated several countries including the US and China to ban the use of antiviral drugs in poultry. Nevertheless, illegal use of antivirals in chicken still occurs, making it necessary to develop a method to detect residues of these drugs in chicken. Even though several methods for this purpose already exist, they generally require derivatization and tedious extraction procedures. A simultaneous determination of 14 antiviral drugs in chicken meat using QuEChERS-UPLC-MS/MS was reported [
Milk can be contaminated with pesticides when cows consume contaminated feed or water, and administration of veterinary drugs to the animals can result in the appearance of residues of antibiotics, hormones, anthelmintics, and other drugs in both milk and meat. Milk is an important component in the diet of children; hence, contamination with xenobiotics is of great concern. Milk is an emulsified fatty product; thus, both hydrophilic and hydrophobic xenobiotics can be present in it, making multiresidue analysis challenging. Therefore, an optimized QuEChERS methodology would save on cost and time when analyzing xenobiotics in milk. Response surface methodology was used to optimize the amount of sorbents (NaOAc, PSA, and C18) used in a QuEChERS-GC-ECD method for the simultaneous determination of 14 pesticides in milk, achieving recoveries >82% for hydrophilic pesticides, although recoveries of four lipophilic pesticides were <80% [
In addition, some QuEChERS-based methods for the analysis of veterinary drugs in milk have focused on particular compounds. Determination of the anthelmintic monepantel in milk using QuEChERS was reported by Kinsella et al. [
The presence of hormone residues in milk is of concern because they have been associated with precocious puberty, breast cancer, and prostate cancer. Such residues occur by the, sometimes illegal, administration of hormones to cows to stimulate milk production. Hormone residues can be detected by ELISA; however, false positives are an issue. The low concentrations at which they occur and binding to proteins also hinder their detection by analytical equipment. A report described using PSA and ZnO nanoparticles as QuEChERS sorbents for the analysis of anabolic steroid and β-agonist residues in milk, using UHPLC-MS/MS [
Aflatoxins are dangerous carcinogenic mycotoxins that can contaminate grains, oilseeds, and spices and can also appear in milk if the cow had consumed contaminated feed. QuEChERS proved to be useful for the analysis of aflatoxins in milk, using UPLC-MS/MS for their detection [
QuEChERS has also been used in combination with other techniques to achieve purer extracts, facilitating the analysis of trace compounds. QuEChERS was used as a pretreatment step prior to capillary LC-MS/MS for determining chloramphenicol, thiamphenicol, and florfenicol in milk [
Effect of sorbent on the recoveries of florfenicol (FF), thiamphenicol (TAP), and chloramphenicol (CAP) from milk samples extracted by QuEChERS, according to data in [
Eggs may contain many of the same xenobiotics found in chicken including antibiotics, hormones, and pesticides; nevertheless, the MRLs may differ as some products that are allowed in birds raised for meat are banned in egg-laying hens. Moreover, eggs are a complex matrix rich in protein and lipids; their lipoproteins may bind to analytes, and foam may be produced during extraction, making sample cleanup and analysis challenging.
Huertas-Perez et al. [
Melamine is a nitrogenated compound used in the manufacture of plastics and has been illegally added to milk to increase its protein content, with nefarious effects on human health as melamine exhibits renal toxicity. Melamine can also be generated as a by-product of the metabolism of cyromazine in hens. Cyromazine is an insecticide added to the feed of egg-laying hens to prevent maggot infestations in their manure; however, residues of both the insecticide and its melamine metabolite require careful monitoring because of their toxicity. Melamine and cyromazine have been extracted using QuEChERS with acidified acetonitrile or a methanol-acetonitrile mixture and determined by HPLC-DAD [
Effects of solvent on the recoveries of melamine and cyromazine from eggs, using a commercial QuEChERS sorbent for fatty samples (QuEChERS 1 = 2 mL MeCN, QuEChERS 2 = 2 mL MeOH, and QuEChERS 3 = 1 mL MeOH + 1 mL MeCN) and comparison with matrix solid-phase dispersion (MSPD), according to data in [
Mycotoxins can contaminate eggs when hens ingest contaminated feed. Because mycotoxins are powerful carcinogens, their presence in food products should be carefully monitored. Mycotoxins have been determined in eggs using QuEChERS-UPLC-MS/MS either with a cleanup step [
The contamination of aqueous ecosystems with pesticides, pharmaceutical waste, heavy metals, and other substances has resulted in the accumulation of xenobiotics in fish, representing a risk to human health. Therefore, effective multiresidue analysis methods are necessary to monitor the presence of these contaminants in fish. Because of their speed, robustness, and environmental friendliness, QuEChERS-based methods have been used to analyze various contaminants in fish, with excellent results.
The most important contaminants in fish are persistent organic pollutants such as organochlorine pesticides and polychlorinated biphenyls, which accumulate in the adipose tissue and have negative effects on human health. A modified QuEChERS method using CaCl2 and PSA and a freezing-out step for removing fats from fish tissue attained good GC-MS recoveries (70%–115%) for both organochlorine pesticides and polychlorinated biphenyls in tilapia, although recoveries in salmon were lower likely because of the high fat content of this fish [
Polycyclic aromatic hydrocarbons (PAHs) are another group of important contaminants in fish. PAHs are combustion by-products that can accumulate in the adipose tissue and exhibit mutagenic and carcinogenic effects. QuEChERS-GC/MS has been successfully used to determine PAHs in fatty fish including herring and salmon [
Recoveries of selected polycyclic aromatic hydrocarbons (PAHs) from fish, attained using QuEChERS with AOAC extraction salt (QuEChERS AOAC), QuEChERS with EN extraction salt (QuEChERS EN), Soxhlet with hexane, and accelerated solvent extraction (ASE) with CH2Cl2 : MeCN (9 : 1), according to data in [
Veterinary drugs are used in fish farming because of the intensity of such operations, in which large numbers of fish are raised in a small space, becoming prone to infection by microorganisms and parasites. QuEChERS has been applied for the determination of malachite green [
For multiclass pesticide analysis in fish muscle, a novel dual d-SPE cleanup step was introduced [
In addition to contaminants derived from human activities, paralytic shellfish poisoning toxins, which are produced by algae and cause severe food poisoning, have also been determined using QuEChERS [
Honey is a complex mixture of sugars and waxes that vary according to the nectar used by the bees to create it, making its analysis challenging. Pesticide contamination of nectar and honey is not only of concern to human health but also may be associated with the phenomenon of disappearance of hives. Therefore, monitoring of pesticide residues in honey is of interest to ensure its safety to consumers and to determine if pesticides are being accumulated and affect beehives. A multiresidue QuEChERS-based method for analyzing pesticides in honey was proposed [
Among pesticides, neonicotinoids are of particular concern because of their harmful effects on bees and their possible role in bee colony collapse. QuEChERS extraction of neonicotinoids from honey was achieved by dissolving honey samples in water and extracting them with acetonitrile, using SPE citrate sorbent for d-SPE; the clean extracts were then analyzed by UPLC-MS/MS, achieving LODs < 2.5 µg/kg [
The presence of antibiotic residues in honey is also of concern. For analyzing nitrofurans and nitroimidazoles in honey, samples were derivatized with acid, QuEChERS extraction was performed without sorbent addition, and the extract was evaporated and reconstituted prior to LC-MS/MS analysis; the validated method complied with European guidelines [
Because honey can also be simultaneously contaminated with various xenobiotics, a multiresidue method able to determine various compound classes would be useful; such a method was recently reported, using a combination of conventional QuEChERS and SPME with both LC-MS/MS and GC-MS/MS for determining more than 100 compounds between pesticides, PAHs, and PCBs [
In addition to contaminants derived from human activities, it is known that honey may become contaminated with natural toxins like alkaloids from various plant species, which is of concern particularly when children consume it; thus, QuEChERS was recently applied to determine both pyrrolizidine and tropane alkaloids in honey [
The QuEChERS methodology has been successfully applied for the analysis of various contaminants in food products of animal origin, yielding high recoveries that are comparably higher than those obtained with other techniques, while decreasing the needs for time and reagents. Nevertheless, to ensure the success of this technique, solvent and sorbent selection is of critical importance. As shown in Table
The QuEChERS methodology has demonstrated to be applicable to the analysis of various xenobiotics including pesticides, hormones, toxins, and antibiotics in animal matrices such as meat, milk, eggs, and honey. QuEChERS exhibits advantages over traditional methods because of its speed, efficiency, and environmental friendliness. Recoveries obtained using QuEChERS tend to be comparable or even higher than those obtained by solvent extraction or SPE, while reducing the need for solvent as well as the analysis time. QuEChERS has also proven to be applicable to the analysis of compounds that are of particular concern in recent times, such as melamine and ractopamine. Therefore, it is expected that new modifications to the QuEChERS methodology will continue to be developed to facilitate the analysis of more veterinary drugs and other xenobiotics in animal products, and the methodology may become a favored choice for the monitoring of these substances in the future.
The authors declare no conflicts of interest.
This research was supported by the Bisa Research Grant of Keimyung University in 2015.