|
| Matrix | Extraction | Clean-up step | Analytes | LC conditions | Chromatographic column | Sensitivity (μg/kg) | References |
| LOD | LOQ |
|
| Cereal biscuits, Cocoa biscuits, minicake, crackers, wholemeal crackers, bread, and wholemeal bread | Methanol/water (80 : 20) mixture | 2% v/v sodium hypochlorite solution treatment | DON-3G | Linear binary gradient with the following solvents: A was made by water (0.5% acetic acid), B was made by 100% methanol (0.5% acetic acid). Gradient elution 0–3 min, isocratic step 10% B; 3–21 min to 40% B; 21–27 min to 60% B; 27–30 min to 10% B; finally, a reequilibration step at 10% B | Kinetex C18 column (2.6 lm; 100 A;150 mm 2.10 mm; Phenomenex, Torrance, CA, USA) | 4 | 11 | [170] |
|
| Corn flakes, corn-based breakfast cereals , corn chips, and tortilla chips | Methanol-acetonitrile-water (25 : 25 : 50, v/v/v) | 10 ml of a combined mixture of 10 ml filtrate and 10 ml phosphate-buffered saline (PBS, 0.2 g KCl, 0.2 g KH2PO4, 1.16 g Na2HPO4, 8 g NaCl, and 1 g NaN3 in 1 L H2O (pH 7.0 with 1N HCl) were added to a FumoniTest™ immunoaffinity column (IAC) | Hydrolyzed fumonisin B1
Hydrolyzed fumonisin B2 | Acetonitrile-methanol (50 : 50, v/v) (Eluent A) and 0.02% aqueous formic acid (v/v) (Eluent B). Gradient elution: 0–1 min 35% A; 1%10 min 60% A; and 10-16 min: maintained 60%. | HPLC MS: A Quatro II tandem mass spectrometer with electrospray ionization (ESI) in positive-ion mode (Micromass, Manchester, UK) interfaced with a HP 1100 LC system (Agilent Technologies, PaloAlto, CA, USA) equipped with Synergi Polar PR column (15 cm, 2 mm, 4 mm) | 0.001
0.0015 | n.d
n.d | [177] |
|
| Maize and maize-based products | Acetonitrile : water 1 : 1 | — | HFB1
HFB2
HFB3 | Water (eluent A) and methanol (eluent B), both acidified with 0.1% formic acid: 0–3 min, isocratic step 100% A, switched to the waste in order to wash out the salts and to focus the analytes on the C18 precolumn cartridge; 3–5 min to 45% B; 5–10 min isocratic 45% B; 10–25 min to 85% B, 25–35 min isocratic 85% B; finally, a reequilibration step at 100% A. | LC-MS/MSColumn C18 XTerra Waters narrow bore (250 × 2.1 mm, 5 μm) equipped with a C18 precolumn cartridge | 20
25
20 | 70
70
70 | [171] |
|
| Gluten-free products | Water/methanol (30 : 70 v/v) | | Hydrolyzed FB1, FB2 and FB3 | A: water and B: methanol, both acidified with 0.2% formic acid: 0–2 min, isocratic step 30% B, and to focus the analytes on the C18 precolumn cartridge; 2–5 min to 45% B; 5–25 min to 90% B; 25–35 min isocratic step 90% B, 35-36 min to 30% B; finally, a reequilibration step at 30% B (initial conditions) for 20 min | LC-MS/MS: C18 XTerraWaters narrow bore (250 mm, 62.1 mm, 5 lm) equipped with a C18 precolumn cartridge | 20 | 70 | [177] |
|
| Raw maize and maize-based products | 10 mL of 2M NaOH | | HFB1
HFB2 | A (0.1% formic acid in water) and B (methanol).
(i) 0∼3.0 min, 40% B; 3.0∼10.0 min, 40%∼100% B;10.0∼11.0 min, 100% B; 11.0∼12.0 min, 00%∼40% B; 12.0∼15.0 min, 40% B | Agilent EclipseXDB-C8 column (150 mm × 4.6 mm, 5 μm i.d., Agilent, Santa Clara, CA, USA) | 6
6 | 23
23 | [173] |
|
| Cereal and maize products | 10 mL of KOH (2M) | — | HFB1 | Water (A) and methanol (B). The gradient started at 40% B; held for 1 min; increased to 86% B in 11 min, held for 2 min; increased to 95% B in 2 min and held for 4 min | LC-MS/MS Gemini C18 analytical column (150 × 4.6 mm, 5 m) preceded by a C18 security guard cartridge (4.0 × 3.0 mm, 5 m), both from Phenomenex® | n.d | [0.5–121] | [176] |
|
| Wheat | MeOH : dichlormethane, 50 : 50 | Strata-XR | DON-3-glucoside (D3G) | MeOH/water, 70 : 30 | QP8000R MS/MSSynergyR fusion 150 × 4.6 × 4 | 0.5 | 1 | [169] |
|
| Malts | ACN : water, 84 : 16 | MycosepR 226 | D3G | MeOH/water | LCQR MS/MS:SynergyR hydroRP 100 × 3 × 4 | 0.5 | 5 | [168] |
|
| Malts | ACN : water, 84 : 16 | — | D3G | MeOH/water | LCQR MS/MSSynergyR hydroRP 100 × 3 × 4 | n.d | [1–2.5] | [178] |
|
