Table 7.
Analytical methods for ibotenic acid and muscimol detection.
| Ref. | Matrix | Separation | Detection | Qualitative/Quantitative | LOD | LOQ | Linearity | Extraction Recovery | Additional Analytical Information |
|---|---|---|---|---|---|---|---|---|---|
| [199] | Mushrooms | GC | MS | Quantitative | NC | NC | NC | NC | Columns: (0.75 m × 2.8 mm) OV-101 and (1.2 m × 2.8 mm) SE-30; Helium flow rate: 20 mL/min; T transfer line: 175 °C |
| [200] | Mushrooms | HPLC | UV (440, 570 nm) | Quantitative | 30 ng | NC | NC | NC | Column: (350 mm × 2.7 mm); RT IBO: 11 min, MUS: 83 min |
| [188] | Mushrooms | HPLC | UV (210 nm) | Quantitative | 1 ppm | NC | NC | <98% | Column: (25 mm × 4.0 mm) IRICA RP-18T; Flow rate: 0.6 mL/min; Mobile phase: H2O/ACN/MeOH (65:20:15; v/v/v) with 2.1 mM sodium dodecyl sulfate + 4 mM H3PO4, isocratic mode |
| [201] | Mushrooms | HPLC | UV (230, 254 nm) | Quantitative | 18 µg/L IBO 0 µg/L MUS |
NC | 50–1000 µg/L IBO 100–3000 µg/L MUS |
NC | Column: (250 mm × 4.6 mm) 5 µm Spherisorb S5 ODS-2; Flow rate: 0.1 mL/min; Mobile phase: 5 mM octylammonium o-phosphate |
| [202] | Mushrooms | HPLC | PDA | Quantitative just of IBO | NC | NC | NC | NC | Preparative column IBO: (115 mm × 13 mm) C18; Flow rate IBO: 0.5 mL/min; RT IBO: 8.2 min; Column MUS: (150 mm × 4.6) Zorbax SB-Aq; Flow rate MUS: 1.0 mL/min; RT MUS: 12.8 min; Mobile phase: H2O/ACN/MeOH (65:20:15; v/v/v) with 2.1 mM sodium dodecyl sulfate + 4 mM H3PO4, isocratic mode |
| HPLC | UV-MS (UV: 254 nm) |
Column: (100 mm × 2.1 mm) 5 µm XTerraTM MS C18; Flow rate: 0.5 mL/min; Mobile phase: H2O/MeOH (19:1; v/v) to ACN/H2O/MeOH (18:1:1; v/v/v) | |||||||
| [203] | Mushrooms | HPLC | ESI-MS/MS (triple Q) (IBO: 159 to 113.1;159 to 42.3 m/z; MUS: 115.1 to 98.1; 115.1 to 67.2; 115.1 to 39.4 m/z) |
Quantitative | NC | NC | NC | NC | Column: (150 mm × 2.1 mm) 5 µm Uptisphère ODB C18; Flow rate: 0.2 mL/min; Mobile phase: 2mM ammonium formiate buffer pH 3 (A), ACN (B) |
| [189] | Mushrooms | GC | MS (SIM: IBO: 257 m/z, MUS: 243 m/z) |
Quantitative IBO/MUS | NC | NC | 10–400 ppm IBO 25–2000 ppm MUS |
NC | Column: (30 m × 0.25 mm) 0.25 µm DB-5 ms; Helium flow rate: 53 mL/min; T injector: 250 °C; Toven: 100 °C |
| [204] | Mushrooms | HPLC | UV (256 nm) | Quantitative | 7.8 ppm IBO 1.4 ppm MUS |
25.9 ppm IBO 4.6 ppm MUS |
40–2500 ppm IBO 25–2500 ppm MUS |
95.4–101.1% | Column: (150 mm × 2.1 mm) 3.5 µm Symmetry C18; Flow rate: 0.2 mL/min; Mobile phase: 10 mM ammonium acetate (A), ACN (B); RT IBO: 25.92 min, MUS: 24.65 min |
| LC | ESI-MS/MS (ion trap) (IBO: 419 to 355; 419 to 235; 419 to 183 m/z; MUS: 347 to 317; 347 to 276; 347 to 226; 347 to 183 m/z) |
Qualitative | 25 ppm | NA | NA | NA | |||
| [158] | Urine | HPLC | ESI-MS (Full-scan mode) |
Qualitative | 50 µg/L IBO 40 µg/L MUS |
NC | NC | 15% IBO 22% MUS |
Column: (150 mm × 2.0 mm) 5 µm Gemini C18; Flow rate: 0.2 mL/min; Mobile phase: 8 mmol/L heptafluorobutyric acid in H2O; RT: IBO 2.6 min, MUS 4.6 min |
| [176] | Urine | GC | MS (Full Scan: 40–400 m/z and SIM: MUS: 113 m/z; IBO: 257 m/z) |
Quantitative | 1 mg/L | NC | 1–15 mg/L | 74% IBO 80% MUS |
Column: (15 m × 0.25 mm) 0.25 µm HP-5MS; Helium flow rate: 1.5 mL/min; T injector: 220 °C; T transfer line: 250 °C |
| [186] | Mushrooms | LC-HILIC | ESI-MS/MS (triple Q) (IBO: 159 to 113.1 m/z; MUS: 115 to 98.1 m/z) |
Quantitative | <10 µg/g | NC | 10–500 µg/g | 84.6–107% | Column: (150 mm × 2.0 mm) 3 µm TSK-GEL Amide-80; Flow rate: 0.5 mL/min; Mobile phase: H2O 0.5% HCOOH (A), ACN 0.5% HCOOH (B) |
| [177] | Serum | LC-HILIC | ESI-MS/MS (triple Q) (IBO: 159 to 113.1 m/z; MUS: 115 to 98.1 m/z) |
Quantitative | 1 µg/L IBO 2.5 µg/L MUS |
NC | 10–1000 µg/L | 87.9–103% | Column: (150 mm × 2.0 mm) 3 µm TSK-GEL Amide-80; Flow rate: 0.5 mL/min; Mobile phase: H2O 0.5% HCOOH (A), ACN 0.5% HCOOH (B) |
| [187] | Mushrooms | Electrophoresis | PDA (214 nm) | Quantitative | 1.5 µg/g IBO 1.8 µg/g MUS |
4.6 µg/g IBO 5.4 µg/g MUS |
2.5–7000 mg/L | 87–95% | Capillary length: 57 cm (75 µm); Running buffer: 25 mM sodium phosphate pH 3 (5:95; v/v) |
| [182] | Urine | Electrophoresis | ESI-MS/MS (triple Q) (SIM and MRM mode) |
Quantitative | 0.15 µg/L IBO 0.05 µg/L MUS |
NC | 10–1000 µg/L | 92.6–95.4% | Capillary length: 100 cm (50 µm); Flow rate: 0.4 mL/min; Sheath liquid: H2O/MeOH/CH3COOH (20/79.65/0.35; v/v/v) |
| [205] | Urine | NMR | - | Quantitative | 30 mg/L IBO 3 mg/L MUS |
NC | 2–417 mg/L IBO 3–278 mg/L MUS |
NC | - |
| [56] | Standard solution | - | PSI-HR-MS/MS (IBO: 159.0397 to 113.0348 m/z MUS: 115.0504 to 98.0241 m/z) |
Qualitative | NA | NA | NA | NA | - |
NA: not applicable; LOD: limit of detection; LOQ: limit of quantification; NC: not communicated; RT: retention time; IBO: ibotenic acid; MUS: muscimol.