Table 1.
Calibration curves, linear ranges, sensitivity, precision, stability, and accuracy for quantitative assay of 20 analytes.
| Analyte | Linearity | LLOQ (μg/mL) | LODa (ng/mL) | Repeatability (RSD, %, n = 6) | Spike recovery % (RSD, %, n = 3) | Stability (RSD, %, n = 6) | |||||
|---|---|---|---|---|---|---|---|---|---|---|---|
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| Range (μg/mL) | Equation | R 2 | Intraday | Interday | High | Middle | Low | ||||
| UPLC-QTOF-MS/MS assay | |||||||||||
| Neomangiferin | 0.05–10 | y = 522.37x – 26,433.83 | 0.9998 | 0.05 | 0.71 | 1.53 | 4.26 | 96.51 (2.62) | 101.76 (1.48) | 105.87 (5.47) | 4.21 |
| Mangiferin | 0.125–50 | y = 701.07x + 49,783 | 0.9993 | 0.125 | 0.33 | 4.25 | 4.62 | 106.72 (0.51) | 102.98 (5.51) | 105.54 (4.30) | 2.72 |
| Isomangiferin | 0.05–25 | y = 430.23x – 8113 | 0.9999 | 0.05 | 0.96 | 4.11 | 5.08 | 107.54 (4.46) | 106.64 (1.60) | 101.15 (0.61) | 3.93 |
| Neoliquiritin | 0.02–25 | y = 341.5x – 7107.5 | 0.9996 | 0.02 | 6.16 | 1.86 | 3.53 | 101.28 (2.46) | 100.07 (5.09) | 99.07 (4.81) | 3.38 |
| Liquiritin | 0.02–50 | y = 612.15x – 3713.8 | 0.9999 | 0.02 | 3.95 | 2.18 | 4.09 | 104.56 (0.50) | 101.05 (3.27) | 102.82 (4.25) | 3.07 |
| Liquiritin apioside | 0.125–100 | y = 431.08x – 46,525 | 0.9997 | 0.125 | 3.76 | 1.94 | 3.82 | 105.23 (0.56) | 105.62 (0.51) | 109.65 (2.11) | 3.63 |
| Isoliquiritin | 0.01–25 | y = 914.32x – 3529.1 | 0.9998 | 0.01 | 1.88 | 2.02 | 3.01 | 102.65 (3.40) | 100.65 (2.25) | 110.38 (0.41) | 1.76 |
| Timosaponin BII | 0.25–100 | y = 203.08x – 33,875 | 0.9995 | 0.25 | 1.25 | 1.73 | 3.73 | 105.67 (5.40) | 101.96 (0.58) | 106.94 (4.28) | 4.77 |
| Glycyrrhizic acid | 0.01–1.25 | y = 343.74x – 3113.7 | 0.9994 | 0.01 | 0.39 | 2.14 | 5.00 | 109.36 (0.90) | 97.30 (4.64) | 100.94 (8.68) | 2.91 |
| Timosaponin AIII | 0.02–25 | y = 144.56x – 489.78 | 0.9993 | 0.02 | 1.25 | 1.69 | 4.01 | 98.08 (2.74) | 97.12 (3.88) | 102.53 (3.24) | 3.34 |
| UPLC-PDA assay | |||||||||||
| Mannose | 0.39–200 | y = 8406.6x – 3645.8 | 0.9997 | 0.39 | 0.10 | 3.52 | 2.92 | 99.50 (4.12) | 96.57 (1.59) | 100.11 (4.42) | 4.39 |
| Rhamnose | 3.91–2000 | y = 1179.3x + 9760.6 | 0.9992 | 3.91 | 0.49 | 3.29 | 2.83 | — | 5.12 | ||
| Glucuronic acid | 0.78–400 | y = 8626.7x – 9639.6 | 0.9997 | 0.78 | 0.39 | 1.22 | 4.00 | — | 3.58 | ||
| Galacturonic acid | 0.78–400 | y = 4388.4x – 24,087 | 0.9993 | 0.78 | 0.33 | 2.22 | 4.01 | 91.97 (1.97) | 103.15 (2.88) | 95.58 (0.73) | 4.18 |
| Glucose | 3.91–2000 | y = 3229.6x + 37,825 | 0.9995 | 3.91 | 0.49 | 4.39 | 2.84 | 107.16 (1.59) | 96.52 (3.70) | 108.35 (1.00) | 2.70 |
| Galactose | 0.78–400 | y = 6392.9x + 6833.8 | 0.9997 | 0.78 | 0.20 | 4.74 | 3.58 | 105.55 (3.23) | 105.43 (4.27) | 93.71 (2.62) | 3.48 |
| Arabinose | 0.39–200 | y = 3040.3x + 6130.3 | 0.9996 | 0.39 | 0.17 | 2.97 | 4.92 | 93.61 (3.09) | 102.16 (4.76) | 107.97 (2.06) | 2.30 |
| Fucose | 3.91–2000 | y = 19,907x + 21,304 | 0.9991 | 3.91 | 0.98 | 3.56 | 4.12 | – | 3.56 | ||
| Sucrose | 105.22 (1.38) | 112.13 (3.21) | 101.19 (1.32) | ||||||||
| Maltotriose | 94.45 (2.99) | 108.85 (5.08) | 113.73 (3.98) | ||||||||
LLOQ = lower limit of quantification; LOD = limit of detection; RSD = relative standard deviation; UPLC-PDA = ultraperformance liquid chromatography coupled with photodiode array detector; UPLC-QTOF-MS = ultra-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry.
a
The LOD unit of UPLC-PDA assay is μg/mL.