Review Article

Dispersive Solid Phase Extraction for the Analysis of Veterinary Drugs Applied to Food Samples: A Review

Table 5

QuEChERS applied to dispersive techniques in the analysis of veterinary drugs in different matrices.

AnalyteMatrixExtraction procedureClean-upTechniqueLimit of detectionRecoveryReference

BAsMilk and ovine muscle10 g of milk simple + 10.0 mL ACN + 5 g MgSO4:NaCl DSPEHPLC-MS/MS 2.2–2.08 µg Kg−1 (milk)108.0–106.0% [89]
The mixture was shaken and centrifuged; the supernatant was cleaned by DMSO solution771.0–746.0 µg Kg−1 (muscle)109.0–108.0%

BZDsEggs3 g of sample + ACN + 4 g of MgSO4/1 g of NaCl/1.0 mL of ammonium formate solution (10.3 M, pH 7.5)
The mixture was centrifuged and diluted with the standard solution CBZ D3
DSPE PSA/MgSO4CE-MS3.0–51.0 μg L−174.0–112.0% [20]

CAP, TAP, and FFMilk and honey2 g sample + 15.0 mL of 1% HAc + 4 g Na2SO4 + 1 g NaCl shaken and centrifuged. Supernatant with 15 g of C18, 0.35 g of C18 endcapped sorbents and 0.5 g of QuE Z-Sep+ QuEChERS Z-Sep+/C18 LC-MS/MS 0.02−0.045 ng g−195.8–100.2% (milk) [53]
The supernatant was evaporated and reconstituted in 0.5 mL of 10% CAN/water95.6–99.3% (honey)

MultiresidueChicken tissueExtraction by SPE, supernatant was added 500 mg (NH2 or PSA), shaken, and centrifuged
An aliquot of sample was evaporated and dissolved in ACN/water
DSPE/NH2/PSALC-MS/MS0.27–444.0 μg g−137.0–89.0%[90]

MultiresidueHoneyA modified QuEChERS without addition of PSA followed by evaporation under vacuum was employed + 4 g of MgSO4 and 1 g NaCl, shaken and centrifuged and reconstituted into 1.0 mL of ammonium formate in MeOH/waterQuEChERSLC-MS/MS0.12–0.74 μg kg−190.9–104.8%[91]

MultiresidueMuscle tissue5 g of sample + 10.0 mL 2% HAc:ACN + 2 g NaCl + 40 g Na2SO4
The mixture was centrifuged and reconstituted in ACN/formic acid
QuEChERS/C18UHPLC-MS/MS0.007–66.715 µg kg−160.0–120.0%[92]

MultiresidueEggs10 g of sample + 1% of acetic acid/ACN/0.1 M Na2EDTA solution, with 4 g of MgSO4/1 g sodium acetate
The mixture was centrifuged and diluted with MeOH/formic acid, 0.05%
PSAUHPLC-MS/MS2.1–220.8 mg kg−170.4–94.8%[51]

MultiresidueMilk10 g of sample + 1% of acetic acid in ACN/0.1 M Na2EDTA solution, with 4 g of MgSO4/1 g of sodium acetate
The mixture was centrifuged and diluted with MeOH/formic acid, 0.01%
DSPE/PSAUHPLC-MS/MS1.0–4.0 mg kg−170.0–110.0%[50]

MultiresidueChicken muscle5 g of the sample + water/1% acetic acid/in a solution of ACN:water
0.5 g of sodium citrate dibasic + 1 g sodium citrate dehydrate and 4 g MgSO4
The mixture was centrifuged and diluted with formic acid 0.1% in ACN:water
PSAUHPLC-MS/S3.0–6.0 μg L−170.0–120.0%[93]

MultiresidueFish muscle5 g of sample + water, in ACN:MeOH solution
4 g of MgSO4/1 g of sodium acetate
The mixture was centrifuged and diluted with mixture 0.1% formic acid in ACN and 0.1% formic acid in water
UHPLC-MS/S7.5 μg kg−169.0–125.0% [88]

MultiresidueFeedstuffs2 g of ground sample + MeOH:ACN
The mixture was centrifuged and the supernatant was diluted with MeOH:0.1% formic acid
DSPE/PSALC-MS/MS0.42–5.74 μg kg−156.7–103.0%[94]

MultiresiduesBovine muscle2 g sample + 10.0 mL of ACN/water, shaken, centrifuged and 10.0 mL of hexane/can. Reconstituted with 0.1% formic acid
Clean-up: hexane; C18; Z-Sep+; Z-Sep (only) and Z-Sep + C18; C18 + hexane; Z-Sep+ + hexane; Z-Sep + hexane; Z-Sep + C18 + hexane
Z-Sep/C18UHPLC-MS/MS70.0–120.0%[55]

MultiresiduesAnimal tissuesDSPE: 2 g sample + 10.0 mL of ACN/water was shaken and centrifuged
The DSPE cleanup with 500 mg endcapped C18 sorbent + 1.5 mL water in 2 g sample, the final extracts equivalence of 0.174 g mL−1 in ≈7 : 3 ACN/water.
DSPE-EMR-LUHPLC-MS/MS 32.0–140.0% (DSPE) [15]
EMR-L: 2 g sample + 10.0 mL ACN/5% formic acid was shaken and centrifuged
5.0 mL of 5 mM NH4HCO2 was added to the EMR-L tube which contains 1 g of the proprietary material and clean-up with 5.0 mL ACN + 2 g MgSO4.
4.0–148.0% (EMR-L)

NSAIDsMilk5 g of sample + 10.0 mL of 5% HAc:ACN, + NH4HCO2 + 4.0 mL of ascorbic acid 0.02 M in HCl 0.24 M + 5 g Na2SO4. The mixture was centrifuged and cleaned with C18-MgSO4 and diluted to 500 μL with 0.1% formic acidQuEChERSHPLC-MS/MS0.4–1.5 μg kg−178.1–97.1%[27]

QNsHoney1 g sample + 30 mM NaH2PO4 buffer pH 7.0 + 5% formic acid in ACN
The mixture was centrifuged and the supernatant was dried under a stream of nitrogen
The residue was diluted with H2O/ACN/formic acid
UHPLC-MS/S0.2–4.1 μg kg−170.1–93.7%[95]

SAsChicken muscle and eggs5 g sample + 5.0 mL water + 10.0 mL ACN: 1% HAc was shaken and 4 g MgSO4 + 1 g NaOAc shaken and centrifuged
Cleaning up MeCN-based and supernatant + 300 mg of Z-Sep+ and once dried was redissolved with 1.0 mL MeOH/water
QuEChERS/PSA/QuE Z-Sep+HPLC-FLD4.66–28.33 μg kg−165.9–88.1%[54]

β2-agonistMeat5 g sample + 4.0 mL of 0.05 M acetate pH 5.2 + 50 μL of β-glucuronidase-arylsulphatase
The supernatant with DVB-NVP-SO3Na, shaken, centrifuged, and dissolved in 0.4 mL of MeOH/water containing 0.1% formic acid
QuEChERSLC-MS/MS0.2–0.9 μg kg−165.0–100.0%[28]

ACN: acetonitrile; BAs: benzimidazole anthelmintics; BZDs: benzimidazoles; CAP: chloramphenicol; CBZ: carbendazim; CE: capillary electrophoresis; DAD: diode-array detection; DSPE: dispersive solid-phase extraction; DMSO: dimethyl sulfoxide; DVB-NVP: divinylbenzene/N-vinylpyrrolidone copolymer; ESI-MS/MS: electrospray ionization tandem mass spectrometry (ESI-MS/MS); EMR-L: enhanced matrix removal for lipids; HPLC: high performance liquid chromatography; FL: fluorescence; FF: florfenicol; LC: liquid chromatography; MeOH: methanol; MgSO4: magnesium sulfate; MS: mass spectrometry; NaCl: sodium chloride; Na2EDTA: ethylenediaminetetraacetic acid disodium salt; NSAIDs: nonsteroidal anti-inflammatory drugs; PSA: primary and secondary amine; QNs: quinolones; SAs: sulfonamide; TAP: thiamphenicol; UHPLC: ultra-high performance liquid chromatography; UV: ultraviolet detection.