Table 7.

Analytical methodologies reported in the scientific literature (2011–2020).

Sample Type	Coccidiostats	Extraction/Purification	Detection and Quantification	LOD (µg/kg)	LOQ (µg/kg)	Accuracy	Precision	Reference
chicken, turkey, eggs, water and feed	Clazuril, Diclazuril, Decoquinate, DNC, Halofuginone, Lasalocid, Maduramicin, Monensin, Narasin, Robenidine, Salinomycin, Semduramicin	Octadecyl sorbent	LC-MS/MS Column: Poroshell EC-C18, 2.7 µm, 2.1 × 150 mm. Mobile phase: (acetonitrile: methanol: 0.01 M ammonium formate at pH 4.0	10 µg/kg	0.2 µg/kg	88%	17.6%	[65]
Milk, Chicken and eggs	Lasalocid, salinomycin, monensin, narasin, madubamycin and nigericin	Acetonitrile extraction followed by alumina SPE clean-up	(SPE)-LC-MS/MS Hypersil Gold column (2.1 × 150 mm, 5 µm)	0.01–0.3 µg/kg	0.4–1 µg/kg	92–97%	-	[68]
Poultry muscle and liver, bovine muscle, liver, and kidney tissues.	Lasalocid, halofuginone, narasin, monensin, semduramicin, ethopabate, robenidine, buquinolate, toltrazuril as its sulfone metabolite, maduramicin, salinomycin, diclazuril, amprolium, decoquinate, dinitolmide, clopidol, and the nicarbazin metabolite DNC (N,N1-bis(4-nitrophenyl)urea)	Methanol (≥99.8%), acetonitrile (≥99.8%), and 2-propanol (≥99.7%)	LC-MS/MS and the LC-QToF/MS Agilent Poroshell 120 EC-C18 analytical column (2.1 × 100 mm, 2.7 µm) held at 55 °C with a 3 μL injection volume of all samples and standards	0.2–91 µg/kg	0.6–305 µg/kg	49–104%	0.3 to 10%	[69]
Eggs	Clazuril, DIC, ROB, NIC, toltrazuril (and its 2 metabolites)	Solid-liquid extraction and purification (SPE)	LC-MS/MS Column Phenomenex C18 (5 µm, 150 mm × 2.1 mm) Mobile phase: 0.1% aqueous formic acid (A) and Ammonium hydroxide (0.08%) (B)	CCα: 2.2−320.0 µg/kg	CCβ: 2.6−350.0 µg/kg	80% (62% was minimum for robenidine and 95% was maximum for toltrazuril)	2.9−14.7% Repeatability: 4.1–13.0% Intra-laboratory reproducibility: 6.4–14.1%	[72]
Fried chicken, non-fried chicken cutlet and chicken muscle	37 compounds belong, including LAS, MAS, MON, NAR, SAL, SEM, DEC, DIC, NIC	Acid extraction (SLE with ethyl acetate and acetonitrile)	LC-MS/MS Column: InertSustainSwift C18 (2.1 mm i.d. × 150 mm, 5 µm; GL Sciences) Mobile phase: 0.1% formic acid in 10 mmol/L ammonium acetate (A) and methanol (B)	Not applicable	0.2–1.0 µg/kg	70–105%	Repeatability: 1–11% Intra-laboratory reproducibility: 1–15%	[70]
Broiler muscle and eggs	LAS, MAD, MON, NAR, SAL, SEM, ROB, DIC, toltrazuril, trimethoprim, clopidol, amprolium, diaveridine and NIC	Acetonityl extraction	LC–QqLIT-MS/MS Column: Poroshell 120 EC-C18 coupled to a C18 column Mobile phase: gradient of water and acetonitrile	10% of MRL	25% of MRL	73–115%	0.4–21%	[73]
Animal muscle (chicken, pork, beef, rabbit) and eggs	LAS, amprolium, MON, NAR, MAD, ROB, DEC, NIC, clopidol, HAL, etopabate, diaveridine, arprinocide, DIC, SEM and nigericin.	Solid-liquid extraction with acetonitrile and dispersive SPE	HILIC-MS/MS Column: ACQUITY UPLC BEH HILIC Mobile phase: acetonitrile (A) and ammonium formate with formic acid (B)	0.004–0.560	0.004–0.560	79.1–118%	Muscle: 5.3–20% Eggs: 6.4–17%	[66]
Chicken, pork, beef and fish muscles; chicken eggs; cow milk; pork offal.	20 compounds, including buquinolate, clopidol, closantel, DEC, diaveridine, DIC, dimetridazole, etopabate, HAL, imidocarb, isometamide, levamisole, metronidazole, NIC	acetonitrile/methanol containing formic acid, sodium cetate and magnesium sulfate; purification with n-hexane saturated with acetonitrile	LC-MS/MS Column: Agilent Poroshell 120SB C18 (2.7 mm, 3.0 mm × 150 mm) Mobile phase: methanol (with 0.1% formic acid) and 5 mM ammonium formate	Not applicable	2–5 µg/kg	Broiler muscle recovery: 75.1–118.9%	Chicken muscle: Intra day accuracy: 1.7–40.5% Interday accuracy: 3.4–43.3%)	[75]
Broiler muscle and eggs	Amprolium, clopidol, DEC, MON, nequinato, toltrazuril, toltrazuril sulfona, e toltrazuril, sulfoxide, DIC, LAS, SAL, HAL, MAD, NAR, NIC, ROB e SEM	Extraction with 20 mL of acetonitrile	LC-HRMS Column: Kinetex C18 Mobile phase: water, acetonitrile and methanol	Eggs: CCα: 2.2–336 µg/kg Chicken muscle: CCα: 2.64–589 µg/kg	Eggs: CCβ: 2.58–401 µg/kg Chicken muscle: CCβ: 3.74–749 µg/kg	Eggs: 94.1–105.8% Chicken muscle: 91.6–105.7%	Eggs: 5.2–21.3% Chicken Muscle: 5.2–20.4%	[74]
Chicken muscle, beef muscle and its derivatives: kidney and liver, eggs, milk and pork fat.	Narasin, salinomycin, lasalocid, maturemycin, monensin and semduramycin.	Extraction with supramolecular solvents and dispersive SPE.	LC-MS/MS Column: Phenomenex Luna C18 Injection volume: 2 µL Mobile phase: formic acid (0.1%) in water (A) and formic acid (0.1%) in methanol (B) Flow: 250 µL/min	0.004–0.07	-	71–112%	14 samples of which 3 samples are non-conforming (pig fat, beef kidney and eggs)	[67]