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. 2017 Jun 26;40(15):3020–3045. doi: 10.1002/jssc.201700184

Table 5.

Chromatographic approaches for 3HAA determination

HPLC‐UV
LOD (μM) CR (μM) Mobile phase composition λ (nm) Application Reference
− up to 660.00 40 mM acetate‐citrate buffer (pH 4.5), 2.5% v/v CH3CN 254 Human urine 123
HPLC‐FD
LOD (μM) CR (μM) Mobile phase composition λex/λem (nm) Application Reference
− − 250 mM (CH3COO)2Zn, 0.9% v/v CH3CN, pH adjusted to 5.8 with CH3COOH 316/420 Human plasma 40
0.001 0.00–10.00 50 mM CH3COOH, 250 mM (CH3COO)2Zn (pH 4.9), 1% v/v CH3CN 320/420 Human serum 94
0.0003 up to 0.50 2 mM hexyl sodium sulfate, 1 mM EDTA, 8% v/v MeOH, 48 mM citric acid, 73 mM NaOH (pH 4.65) 311/414 Rat plasma 157
0.0003 up to 0.50 2 mM hexyl sodium sulfate, 1 mM EDTA, 1.5% v/v MeOH, 48 mM citric acid, 73 mM NaOH (pH 4.45) 311/414 Rat brain 157
0.001 0.005–0.05 90% v/v sodium acetate buffer (pH 5.5), 10% v/v MeOH 316/420 Rat brain 85
HPLC‐ED
LOD (μM) CR (μM) Mobile phase composition Application Reference
0.030 −

  • 50 mM H3PO4, 50 mM citric acid, 60 μM EDTA, 8 mM heptane sulfonic acid, 2 mM NaCl, 5% v/v MeOH

  • pH adjusted to 3.1 with KOH

 Human plasma 44, 46
0.005 0.004–97.95 50 mM sodium phosphate‐acetate buffer (pH 4.1), 10% v/v MeOH, 0.42 mM octanesulphonic acid Rat brain 91
LC/MS or LC/MS‐MS
LOD (μM) CR(μM) Mobile phase composition Monitored ions / transitions (m/z) Application Reference
0.002 0.0005– 0.40 A: 650 mM CH3COOH, B: 100 mM heptafluorobutyric acid. C: 90% v/v CH3CN in H2O 154.1 > 80.0 Human plasma 86

  • 0.003.00

  • 0.0015

  • 0.0008–1.50

  • 0.0008–1.54

 A: 0.1% v/v CH3COOH, B: 100% MeOH 154 > 136 > 108

  • Human serum

  • Human CFS

 2
0.1 0.10–10.00 A: 5 mM CH3COONH4, 0.01% v/v TCA, B: 100% MeOH 154 > 80

  • Human glioma cells

  • Culture medium

 121
0.003 0.005–10.00 A: 0.1% v/v HCOOH in H2O, B: 0.1% v/v HCOOH in CH3CN 154.2 > 80.0

  • Human serum

  • Human urine

  • Cell culture

 111
0.002 0.002–3.26 A: 0.1% v/v HCOOH in H2O, B: 0.1% v/v HCOOH in H2O 387 Human urine 140
− − A: 0.1% v/v HCOOH in H2O, B: 0.1% v/v HCOOH in CH3CN 154.2 > 80 Rat hepatocytes 110
0.003 − A: 28% v/v 0.4 M CH3COONH4, 32% v/v MeOH, 40% v/v CH3CN, B: 32% v/v MeOH, 68% v/v CH3CN 383 > 387 > 389 Culture medium 127

LOD, limit of detection; CR, calibration range; λ, wavelength; λex, excitation wavelength; λem, emission wavelength.