Review Article

Application of QuEChERS for Determining Xenobiotics in Foods of Animal Origin

Table 1

Summary of applications of QuEChERS for the analysis of xenobiotics in animal products.

MatrixAnalytesQuEChERS methodAnalytical methodRef.

Goat’s milk and sheep muscleMonepantel and its sulfone metaboliteMilk (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[11]

Beef muscleCephalosporinsHomogenized 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[3]

Meat and bovine fatChlorfenvinphos, fipronil, and cypermethrinFor 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[12]

BaconNitritesComminuted 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[13]

Meat productsPolychlorinated 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[14]

Sheep meatChlorinated hydrocarbon and synthetic pyrethroidsHomogenized 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[15]

PorkRactopamineGround 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[16]

PorkMethenamineHomogenized 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[17]

ChickenAmantadine and rimantadineHomogenized 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[18]

ChickenAntiviral drugs and relevant metabolitesHomogenized 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[19]

ChickenVeterinary drugsHomogenized 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[20]

ChickenSulfonamidesHomogenized 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 analysisHPLC-DAD[4]

Milk and honeyChloramphenicol, thiamphenicol, and florfenicolSample (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[21]

MilkAnabolic steroids and agonistsMilk (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[22]

Yogurt and milkHerbicides (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[23]

MilkPesticidesMilk (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[24]

MilkPesticidesMilk (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[25]

Raw milk (cow, goat, and buffalo milk)Steroid hormonesMilk (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[26]

MilkSulfonamidesMilk (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[27]

EggsAflatoxins B1, G1, B2, G2, zearalenone, and its metabolitesHomogenized 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[28]

EggsMelamine and cyromazineHomogenized 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[29]

EggsMelamine and cyromazineHomogenized 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[30]

EggsMycotoxinsHomogenized 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[31]

Eggs and egg productsPesticidesHomogenized 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[32]
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.

Eggs, chicken, and porkPhorate and its metabolitesHomogenized 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[33]

Fish (tilapia and salmon)Organochlorine pesticides and polychlorinated biphenylsHomogenized 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[34]

FishOrganochlorine pesticidesHomogenized 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[35]

High-fat smoked salmonParent and substituted polycyclic aromatic hydrocarbonsFour 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[36]

Fish muscle and liver tissuesPersonal 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[37]

Fish (carp and sturgeon)Organochlorine and organophosphate pesticidesHomogenized 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[38]

Fish (catfish)PCBsHomogenized 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[39]

FishQuinolonesHomogenized 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[40]

FishOrganochlorine pesticidesHomogenized 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[41]

BivalvesPharmaceuticalsFrozen-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[42]

BivalvesParalytic shellfish poisoning toxinsHomogenized 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[43]

HoneyNitrofuran metabolites and nitroimidazoleHoney (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[44]

HoneyPesticidesHoney (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[45]

HoneyPesticidesHoney (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[46]

HoneyPesticides, PAHs, and PCBsHoney (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[47]

HoneyPyrrolizidine and tropane alkaloidsHomogenized 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[48]