Table 1.
Application of sorbent-based microextraction techniques for isolation of natural toxins in food samples (2009–2019).
| Food Matrix (Amount) | Analytes | Sample Pretreatment | Microextraction Technique | Analysis | Recovery (%) | LOD | Ref. |
|---|---|---|---|---|---|---|---|
| Cereal flours (2 g) | AF (B1, B2, G1, G2) | Extraction with 10 mL of MeOH/phosphate buffer (80/20, v/v, pH 5.8). Evaporation to dryness and reconstitution with 4 mL of phosphate buffer. An aliquot of the extract (2 mL) subject to microextraction. | SPME Sorbent: Commercial fibers Elution: 0.1 mL MeOH |
HPLC-FLD | 49–59 | 0.035-0.2 μg/Kg | [34] |
| Nuts, cereals, dried fruits and spices (0.5 g) | AF (B1, B2, G1, G2) | Extraction with 1 mL of MeOH/H2O (80/20, v/v). An aliquot of the extract (0.1 mL) mixed with 0.1 mL of 50 mM Tris buffer and brought to a total volume of 1 mL with H2O before microextraction. | In-tube SPME * Sorbent: SUPEL-Q PLOT capillary |
HPLC-MS | 81–109 | 0.0021-0.0028 μg /L | [35] |
| Fruit juice and dried fruit (1 mL) | PAT | - | In-tube SPME * Sorbent: Carboxen-1006 PLOT capillary |
HPLC-MS | > 92 | 0.023 μg /L | [36] |
| Nut and grain samples (0.5 g) | OTA, OTB | Extraction with 1 mL of MeOH/H2O (80/20, v/v). Defatted with 3 mL hexane, supernatant discarded. An aliquot of the clean extract (0.1 mL) brought to a total volume of 1 mL with H2O before microextraction. | In-tube SPME * Sorbent: Carboxen-1006 PLOT capillary |
HPLC-MS | 88 | 0.089-0.092 μg /L | [37] |
| Wine (0.05 mL) | OTA | - | In-tube SPME * Sorbent: Luna C18 particles |
HPLC-MS/MS | 61–73 | 0.02 μg/L | [38] |
| Powdered infant milk (3 mL) and mineral waters (50 mL) | ZEN, α-ZAL, β-ZAL, α-ZEL, β-ZEL, ZAN | Extraction of milk samples with 0.15 mL acetic acid and 6 mL ACN. Evaporation up to 2.5 mL and reconstitution with H2O to 25 mL, pH adjusted to 3.0 before microextraction. | µ-dSPE Sorbent: 80 mg of MWCNTs Elution: 30 mL MeOH/Acetone (1/1, v/v) |
HPLC-MS/MS | 77–120 | 0.05–2.02 µg/L | [39] |
| Peach seed, milk powder, corn flour (0.2 g) and beer (0.2 mL) | AF (B1), OTB, T-2, OTA, ZEN | Microwave assisted extraction of solid samples with 0.2 g NaCl and 5 mL MeOH/H2O (70/30, v/v). An aliquot of the extract (0.2 mL) brought to a total volume of 5 mL with H2O before microextraction. Liquid samples diluted with H2O up to 5 mL before microextraction. |
µ-dSPE Sorbent: 12.5 µg zirconia nanoparticles Elution: 0.1 mL MeOH |
UHPLC-MS/MS | 84–105 | 0.0022–0.017 µg/L 0.0036–0.033 μg/Kg |
[40] |
| Coffee (10 g) and grape juice (10 mL) | OTA | Extraction of coffee samples with 100 mL of carbonate. An aliquot of the extract (10 mL) adjusted to pH 1.5 before microextraction. Grape juice samples adjusted to pH 1.5 before microextraction. |
µ-SPE Sorbent: 15 mg AFFINIMIPTM OTA Elution: 0.25 mL MeOH/Acetic acid (98:2, v/v) |
HPLC-FLD | 91–101 | 0.02–0.06 μg/Kg | [41] |
| Wine (0.35 mL) | OTA | - | MEPS Sorbent: 4 mg C18 sorbent Elution: 0.05 mL ACN/2% Acetic Acid (90/10, v/v) |
HPLC-FLD | 76–108 | 0.08 μg/L | [42] |
* Elution performed with mobile phase (online system); ACN: Acetonitrile; AF: Aflatoxin; F: Fumonisin; HPLC-FLD: High performance liquid chromatography coupled to fluorescence; HPLC-MS/MS: High performance liquid chromatography coupled to tandem mass spectrometry; HPLC-MS: High performance liquid chromatography coupled to mass spectrometry; MeOH: Methanol; MEPS: Microextraction by packed sorbent; MWCNTs: Multiwalled carbon nanotubes; OTA: Ochratoxin A; OTB: Ochratoxins B; PAT: Patulin; SPME: Solid-phase microextraction; T-2: T-2 toxin; UHPLC-FLD: Ultra High performance liquid chromatography coupled to fluorescence; UHPLC-MS: Ultra High performance liquid chromatography coupled to tandem mass spectrometry; ZAL: Zearalanol; ZAN: Zearalanone; ZEL: Zearalenol; ZEN: Zearalenone; µ-dSPE: Micro-dispersive solid-phase extraction; µ-SPE: Micro-solid-phase extraction.