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. 2020 Dec 11;13(12):454. doi: 10.3390/ph13120454

Table 2.

Analytical methods for orellanine detection.

Ref. Matrix Separation Detection Qualitative/Quantitative LOD LOQ Linearity Extraction Recovery Additional Analytical Information
[14] Mushrooms TLC UV Qualitative NA NA NA NA -
[49] Mushrooms TLC UV (254 nm) Qualitative NA NA NA NA -
[50] Mushrooms, mouse serum and kidney HPLC Electrochemistry
(Working electrode: glassy carbon TL-5A; Reference electrode: Ag/AgCl; Working potential: 900 mV)
Quantitative 500 pg NC 50–500 ng on column Alleged to 100% on overloaded mouse serum and directly injected, 25% for mouse kidney Column: (200 mm × 4.6) 5 µm Nucleosil C18; Flow rate: 2 mL/min; Mobile phase: 0.05 citrate-phosphate buffer pH 4.5, 15.4% MeOH and PIC B6 1-hexane sulphonic acid 5 mM
[21] Mushrooms TLC Spectrofluorometry
excitation = 396 nm; λemission = 447 nm)
Quantitative NC NC NC NC -
HPLC MS Qualitative NA NA NA NA
- NMR Qualitative NA NA NA NA
[22] Mushrooms - Polarography
(Working electrode: dropping mercury; Reference electrode: saturated calomel)
Qualitative NA NA NA NA -
[51] Mushrooms HPLC UV (260, 290 nm) Quantitative 40–50 pg on column NC 5–500 ng on column NC Columns: (150 mm × 4.6) 5 µM Rosil CN and (150 mm × 3.9) 5 µM µBondapak C18; Flow rate: 0.5 mL/min and 0.8 mL/min; Mobile phase: H3PO4 pH 1 and H3PO4 pH/ACN (94/6 v/v); 1-octane-sulphonic acid 2.5 Mm; RT: 4.43 min and 6.58
[24] Biological fluids and renal biopsy TLC Spectrofluorometry in 2D
excitation = 399 nm; λemission = 447 nm)
Quantitative 10 ng NC NC NC -
[28] Mushrooms TLC Spectrofluorometry
excitation = 400 nm; λemission = 450 nm)
Quantitative 15 ng deposit NC NC NC -
Electrophoresis Spectrofluorometry
excitation = 400 nm; λemission = 450 nm)
Quantitative 25 ng deposit NC NC NC
- ESR Quantitative 5000 ng NC NC NC
[41] Urine, blood and renal biopsy TLC UV (366 nm) Semi quantitative ≈ 10 ng NC NC NC -
[52] Mushrooms TLC UV (365 nm) Semi quantitative ≈ 50 ng deposit NC NC NC -
HPLC Photodiode (288 nm) Quantitative NC NC NC NC Preparative column: (115 mm × 13 mm) C18; Flow rate: 1 mL/min; Mobile phase: ACN/H2O (5/95 v/v) pH 1 1% TFA; RT: 6.5 min
HPLC ESI-MS Quantitative NC NC NC NC Flow rate: 10 µL/min direct MS source
[10] Mushrooms and rat plasma HPLC ESI-MS/MS (triple Q)
(253 to 191; 253 to 219; 253 to 163 m/z)
Quantitative 4.9 µg/L NC 4.9–5000 µg/L ≈ 91% mushrooms
≈ 60% plasma
Column: (50 mm × 2.1 mm) 1.8 µm Eclipse Plus C18 RRHD; Flow rate: 0.2 mL/min; Mobile phase: 4 mM ammonium formate pH 2.5 (A), MeOH 0.2% HCOOH (B)
ESI-MS/MS (QTOF) Quantitative 4.9 µg/L NC 4.9–5000 µg/L Flow rate: 0.2 mL/min; Mobile phase: 5 mM ammonium formate/MeOH (90/10; v/v) 0.02% HCOOH (A), 5 mM ammonium formate in MeOH 0.02% HCOOH (B)
[53] Rat gastric content HPLC (−) ESI-MS/MS (triple Q)
(Scan range: 120–600 m/z)
Quantitative NC NC NC NC Column: (50 mm × 2.1 mm) 2 µm Ascentis Express C18; Flow rate: 0.25 mL/min; Mobile phase: H2O 0.1 N HCOOH (A), ACN (B)
[54] Rat gastric content GC MS with Supersonic Molecular Beam Qualitative NC NA NA NA Column: (4 m × 0.25 mm ID), 0.1 µm VF-5HT; Flow rate: 8 mL/min; T injector: 200 °C; GC oven: 120–300 °C at 30 °C/min
[26] Mushrooms HPLC UV–visible (295 nm) Quantitative 17000 ng/g NC 17000–680000 ng/g 78.3% Column: (150 mm × 4.6 mm) 3 µm PLRP-S C18; Flow rate: 0.3 mL/min; Mobile phase: 4 mM ammonium acetate (A), MeOH (B)
ESI-MS/MS (triple Q)
(253 to 163; 253 to 191; 253 to 219; 253 to 236 m/z)
Quantitative 30 ng/g NC 6800–13600 ng/g 85.0% Column: (250 mm × 4.1 mm) 10 µm Hamilton PRP-1; Flow rate: 0.4 mL/min; Mobile phase: H2O 1% HCOOH (A), ACN (B)
[55] Mice kidney HPLC UV–visible Quantitative NC 10 µg/g of tissue 15–50 µg/g of tissue NC -
HPLC ESI-MS/MS (triple Q)
(235 to 236 m/z)
Quantitative 20 ng/g NC NC 91%
[56] Standard solution - PSI-HR-MS/MS
(253.0468 to 219.0404 m/z)
Qualitative NA NA NA NA -

NA: not applicable; LOD: limit of detection; LOQ: limit of quantification; NC: not communicated.