Table 6.
Summary of methodologies that applied QuEChERS protocols for the analysis of TAs in foods.
| Analyte | Sample (Amount) | Extraction Conditions | Clean-Up Conditions | Other Treatments | Recovery (%) | [Ref.] |
|---|---|---|---|---|---|---|
| At, Sc + others (pyrrolizidine alkaloids) |
Honey (1.5 g) | 10 mL H2SO4 (0.1 M) + 0.5 g of zinc dust + agitation (1 h 30 min) + centrifuged (10 min, 3700 g) = supernatant + 10 mL ACN + Q-Sep QuEChERS extraction salts: MgSO4 (4 g), C6H5Na3O7 2H2O (1 g), C6H6Na2O7 1.5 H2O (0.5 g), NaCl (1 g) + shaken (4 min) + centrifuged |
PSA (0.15 mg), MgSO4 (0.9 g). Vortex + centrifuged |
Evaporated under vacuum at 45 °C + reconstituted in ACN/H2O (0.1% FA) (13:87, v/v) |
101–104 At 96–109 Sc |
[5] |
| At, Sc | Buckwheat, buckwheat flour and pasta, soy, wheat, amaranthus grain, chia seeds, peeled millet (5 g) |
10 mL H2O + vortex (1 min) + 10 mL of ACN with 1% FA + vortex (2 min) + Na2SO4 (4 g) + NH₄CH₃CO₂ (1 g) + centrifuged (5 min, 5000 rpm) |
PSA (25 mg), GBC (25 mg). Vortex (1 min) + centrifuged (5 min, 5000 rpm) |
Diluted with H2O + filtered | 66–92 At 50–88 Sc |
[22] |
| Sc, L-hyoscyamine + other (sparteine) | Porcine muscle (2 g) Egg and milk (2 mL) |
0.1 mL EDTA + 10 mL of ACN with 0.5% TFA + vortex 5 min + MgSO4 (4 g) + NaCl (1 g) + C6H5Na3O7 2H2O (1 g) + C6H6Na2O7·1.5 H2O (0.5 g) + vortex (5 min) + centrifuged (10 min, 2600 g) |
C18 (0.15 g), MgSO4
(0.9 g) Vortex (5 min) + centrifuged (10 min, 2600 g) |
Evaporated with N2 at 45 °C + reconstituted in MeOH + vortex + centrifuged + filtered |
83–99 At 74–99 Sc |
[30] |
| At, Sc + 9 TAs | Honey (2.5 g) | 10 mL MeOH/ H2O/FA (75:25:0.4, v/v/v) + agitation (30 min) + centrifuged (10 min, 5000 rpm) |
MgSO4 (0.3 g), GBC (0.05 g). Vortex (1 min) + centrifuged (10 min, 5000 rpm) |
Filtered | 71–120 TAs 85–103 At 116–120 Sc |
[32] |
| At, Sc | Wheat, corn, rice, oat and millet flours, mixed cereals flours, infant cereals, cereal-based products (5 g) |
10 mL H2O + shaken + 10 mL of ACN with HAC (95:5, v/v) + agitation (30 min) + QuEChERS salt mixture: NaCl (1 g) + MgSO4 (4 g) + shaken + centrifuged (10 min, 3500 rpm) = 5 mL + hexane + shaken + centrifuged (1 min, 4000 g) |
The hexane phase was discarded | Evaporated with N2 at 40 °C + reconstituted in MeOH + sonicated + diluted with H2O + vortex + centrifuged |
95–107 At 87–118 Sc |
[19] |
| At, Sc | Spinach-based products (10 g) |
10 mL of ACN + NaCl (1 g) + MgSO4 (4 g) + C6H5Na3O7 2H2O (1 g) + C6H6Na2O7 1.5 H2O (0.5 g) + shaken (1 min) + centrifuged (5 min, 3500 rpm) = 5 mL |
PSA (0.25 mg), MgSO4 (0.75 g). Shaken (30 s) + centrifuged (5 min, 3500 rpm) |
Diluted with H2O + Filtered | 94–103 At 91–98 Sc |
[29] |
Abbreviations: ACN: acetonitrile. At: atropine. DSPE: dispersive solid phase extraction. EDTA: ethylenediaminetetraacetic acid. FA: formic acid. GBC: graphitized black carbon. HAC: acetic acid. MeOH: methanol. PSA: primary secondary amine. Sc: scopolamine. TAs: tropane alkaloids. TFA: trifluoroacetic acid.