Chinese Journal of Chromatography ›› 2020, Vol. 38 ›› Issue (6): 672-678.DOI: 10.3724/SP.J.1123.2019.11008
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CEN Jianbin, LIANG Zhisen, OU Shuojun, HUANG Jiale, LI Xiuying, LIN Qinglan, CHEN Yuzhen, LIU Xinjie, LIN Senyu(
)
Received:2019-11-11
Online:2020-06-08
Published:2020-12-10
Contact:
LIN Senyu
CEN Jianbin, LIANG Zhisen, OU Shuojun, HUANG Jiale, LI Xiuying, LIN Qinglan, CHEN Yuzhen, LIU Xinjie, LIN Senyu. Simultaneous determination of five baicaleins in healthy product tablets by dispersive solid-phase extraction-high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2020, 38(6): 672-678.
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URL: https://www.chrom-china.com/EN/10.3724/SP.J.1123.2019.11008
Fig. 1 Chemical structures of the five baicaleins
| Compound | Retention time/min | Ionization model | Precursor ion (m/z) | Product ion (m/z) | Collision energy/eV | RF lens/V |
| * Quantitative ion. | ||||||
| Scutellarein | 10.1 | ESI+ | 287.0 | 123.0* | 32.6 | 135.9 |
| 169.1 | 29.2 | 135.9 | ||||
| 4′-Hydroxywogonin | 12.0 | ESI+ | 301.1 | 286.0* | 23.1 | 139.0 |
| 195.1 | 36.2 | 139.0 | ||||
| Norwogonin | 12.4 | ESI+ | 271.1 | 169.0* | 29.4 | 149.0 |
| 115.1 | 45.6 | 149.0 | ||||
| Baicalein | 12.7 | ESI+ | 271.1 | 123.0* | 31.5 | 141.0 |
| 253.0 | 24.3 | 141.0 | ||||
| Wogonin | 14.4 | ESI+ | 285.1 | 270.0* | 22.5 | 126.8 |
| 151.1 | 44.0 | 126.8 | ||||
Table 1 Parameters for mass spectrometric analysis of the five analytes
| Compound | Retention time/min | Ionization model | Precursor ion (m/z) | Product ion (m/z) | Collision energy/eV | RF lens/V |
| * Quantitative ion. | ||||||
| Scutellarein | 10.1 | ESI+ | 287.0 | 123.0* | 32.6 | 135.9 |
| 169.1 | 29.2 | 135.9 | ||||
| 4′-Hydroxywogonin | 12.0 | ESI+ | 301.1 | 286.0* | 23.1 | 139.0 |
| 195.1 | 36.2 | 139.0 | ||||
| Norwogonin | 12.4 | ESI+ | 271.1 | 169.0* | 29.4 | 149.0 |
| 115.1 | 45.6 | 149.0 | ||||
| Baicalein | 12.7 | ESI+ | 271.1 | 123.0* | 31.5 | 141.0 |
| 253.0 | 24.3 | 141.0 | ||||
| Wogonin | 14.4 | ESI+ | 285.1 | 270.0* | 22.5 | 126.8 |
| 151.1 | 44.0 | 126.8 | ||||
Fig. 2 Extracted ion chromatograms of the five analytes on Hypersil GOLD column
Fig. 3 Effect of different extract solvents on average recoveries of the five analytes (n=6)
Fig. 4 Effect of different dosages of acetone on average recoveries of the five analytes (n=6)
| Compound | Average recoveries/% | |||||||||||||
| GCB/mg | PSA/mg | C18/mg | ||||||||||||
| 10 | 25 | 50 | 10 | 25 | 50 | 10 | 25 | 50 | 75 | 100 | 125 | |||
| Scutellarein | 0.00 | 0.00 | 0.00 | 0.00 | 0.00 | 0.00 | 95.9 | 95.3 | 95.5 | 97.4 | 46.5 | 46.5 | ||
| 4′-Hydroxywogonin | 1.67 | 1.52 | 0.321 | 32.3 | 11.1 | 3.50 | 104 | 103 | 103 | 104 | 98.7 | 98.7 | ||
| Norwogonin | 0.00 | 0.00 | 0.00 | 0.00 | 0.00 | 0.00 | 101 | 100 | 101 | 101 | 83.3 | 82.7 | ||
| Baicalein | 0.00 | 0.00 | 0.00 | 0.00 | 0.00 | 0.00 | 85.9 | 85.1 | 85.4 | 87.5 | 62.7 | 63.2 | ||
| Wogonin | 2.86 | 1.84 | 0.680 | 91.4 | 88.3 | 78.3 | 98.5 | 100 | 99.7 | 101 | 97.5 | 99.1 | ||
Table 2 Effects of three kinds of adsorbents on average recoveries of the five analytes (n=6)
| Compound | Average recoveries/% | |||||||||||||
| GCB/mg | PSA/mg | C18/mg | ||||||||||||
| 10 | 25 | 50 | 10 | 25 | 50 | 10 | 25 | 50 | 75 | 100 | 125 | |||
| Scutellarein | 0.00 | 0.00 | 0.00 | 0.00 | 0.00 | 0.00 | 95.9 | 95.3 | 95.5 | 97.4 | 46.5 | 46.5 | ||
| 4′-Hydroxywogonin | 1.67 | 1.52 | 0.321 | 32.3 | 11.1 | 3.50 | 104 | 103 | 103 | 104 | 98.7 | 98.7 | ||
| Norwogonin | 0.00 | 0.00 | 0.00 | 0.00 | 0.00 | 0.00 | 101 | 100 | 101 | 101 | 83.3 | 82.7 | ||
| Baicalein | 0.00 | 0.00 | 0.00 | 0.00 | 0.00 | 0.00 | 85.9 | 85.1 | 85.4 | 87.5 | 62.7 | 63.2 | ||
| Wogonin | 2.86 | 1.84 | 0.680 | 91.4 | 88.3 | 78.3 | 98.5 | 100 | 99.7 | 101 | 97.5 | 99.1 | ||
| Compound | K values | ||
| Sea cucumber oyster health tablet | Tabletting candy | Vitamin tablet | |
| Scutellarein | 1.19 | 0.86 | 0.83 |
| 4′-Hydroxywogonin | 0.47 | 1.76 | 9.07 |
| Norwogonin | 2.70 | 2.27 | 2.24 |
| Baicalein | 1.19 | 1.14 | 1.11 |
| Wogonin | 1.20 | 3.28 | 0.86 |
Table 3 K values of matrix effects in three sample matrices
| Compound | K values | ||
| Sea cucumber oyster health tablet | Tabletting candy | Vitamin tablet | |
| Scutellarein | 1.19 | 0.86 | 0.83 |
| 4′-Hydroxywogonin | 0.47 | 1.76 | 9.07 |
| Norwogonin | 2.70 | 2.27 | 2.24 |
| Baicalein | 1.19 | 1.14 | 1.11 |
| Wogonin | 1.20 | 3.28 | 0.86 |
| Compound | Calibration curve | Linear range/ (μg/L) | Correlation coefficient | Limit of detection/ (μg/kg) | Limit of quantification/ (μg/kg) |
| Y: peak area of quantitative ion; X: mass concentration, μg/L. | |||||
| Scutellarein | Y=66.41X-46.24 | 1.0-400.0 | 0.9980 | 10.0 | 30.0 |
| 4′-Hydroxywogonin | Y=6804X-667.5 | 0.05-400.0 | 0.9954 | 0.5 | 2.0 |
| Norwogonin | Y=36.86X-44.45 | 5.0-400.0 | 0.9987 | 40.0 | 120.0 |
| Baicalein | Y=379X-125 | 1.0-400.0 | 0.9963 | 10.0 | 30.0 |
| Wogonin | Y=5259X-163.1 | 0.05-400.0 | 0.9966 | 0.5 | 2.0 |
Table 4 Linear relationships, LODs and LOQs of the five analytes in blank matrix of tabletting candy
| Compound | Calibration curve | Linear range/ (μg/L) | Correlation coefficient | Limit of detection/ (μg/kg) | Limit of quantification/ (μg/kg) |
| Y: peak area of quantitative ion; X: mass concentration, μg/L. | |||||
| Scutellarein | Y=66.41X-46.24 | 1.0-400.0 | 0.9980 | 10.0 | 30.0 |
| 4′-Hydroxywogonin | Y=6804X-667.5 | 0.05-400.0 | 0.9954 | 0.5 | 2.0 |
| Norwogonin | Y=36.86X-44.45 | 5.0-400.0 | 0.9987 | 40.0 | 120.0 |
| Baicalein | Y=379X-125 | 1.0-400.0 | 0.9963 | 10.0 | 30.0 |
| Wogonin | Y=5259X-163.1 | 0.05-400.0 | 0.9966 | 0.5 | 2.0 |
| Compound | Added/ (μg/kg) | Sea cucumber oyster health tablet | Tabletting candy | Vitamin tablet | |||||
| Recovery/% | RSD/% | Recovery/% | RSD/% | Recovery/% | RSD/% | ||||
| Scutellarein | 30 | 96.3 | 3.16 | 96.2 | 3.58 | 95.5 | 3.66 | ||
| 150 | 96.8 | 2.18 | 96.2 | 4.17 | 96.1 | 4.08 | |||
| 300 | 97.9 | 2.48 | 95.6 | 3.15 | 99.6 | 3.15 | |||
| 4′-Hydroxywogonin | 2 | 89.4 | 3.18 | 88.5 | 4.02 | 93.1 | 2.57 | ||
| 10 | 106.5 | 4.27 | 100.2 | 4.00 | 97.9 | 0.97 | |||
| 20 | 101.7 | 4.02 | 98.7 | 3.85 | 101.5 | 3.61 | |||
| Norwogonin | 120 | 100.3 | 4.52 | 89.8 | 3.57 | 102.3 | 3.14 | ||
| 600 | 104.5 | 4.03 | 95.4 | 4.02 | 102.8 | 4.03 | |||
| 1200 | 99.9 | 4.12 | 103.7 | 4.32 | 99.1 | 2.58 | |||
| Baicalein | 30 | 83.1 | 2.15 | 86.8 | 2.16 | 86.0 | 3.18 | ||
| 150 | 90.1 | 1.59 | 91.3 | 2.84 | 89.4 | 3.33 | |||
| 300 | 89.4 | 3.01 | 89.4 | 3.55 | 88.0 | 4.20 | |||
| Wogonin | 2 | 95.8 | 4.12 | 99.8 | 3.18 | 102.9 | 4.12 | ||
| 10 | 99.7 | 4.51 | 104.3 | 2.58 | 101.3 | 2.51 | |||
| 20 | 99.1 | 3.79 | 97.4 | 3.10 | 99.6 | 3.15 | |||
Table 5 Recoveries and precisions of the five analytes spiked in samples (n=6)
| Compound | Added/ (μg/kg) | Sea cucumber oyster health tablet | Tabletting candy | Vitamin tablet | |||||
| Recovery/% | RSD/% | Recovery/% | RSD/% | Recovery/% | RSD/% | ||||
| Scutellarein | 30 | 96.3 | 3.16 | 96.2 | 3.58 | 95.5 | 3.66 | ||
| 150 | 96.8 | 2.18 | 96.2 | 4.17 | 96.1 | 4.08 | |||
| 300 | 97.9 | 2.48 | 95.6 | 3.15 | 99.6 | 3.15 | |||
| 4′-Hydroxywogonin | 2 | 89.4 | 3.18 | 88.5 | 4.02 | 93.1 | 2.57 | ||
| 10 | 106.5 | 4.27 | 100.2 | 4.00 | 97.9 | 0.97 | |||
| 20 | 101.7 | 4.02 | 98.7 | 3.85 | 101.5 | 3.61 | |||
| Norwogonin | 120 | 100.3 | 4.52 | 89.8 | 3.57 | 102.3 | 3.14 | ||
| 600 | 104.5 | 4.03 | 95.4 | 4.02 | 102.8 | 4.03 | |||
| 1200 | 99.9 | 4.12 | 103.7 | 4.32 | 99.1 | 2.58 | |||
| Baicalein | 30 | 83.1 | 2.15 | 86.8 | 2.16 | 86.0 | 3.18 | ||
| 150 | 90.1 | 1.59 | 91.3 | 2.84 | 89.4 | 3.33 | |||
| 300 | 89.4 | 3.01 | 89.4 | 3.55 | 88.0 | 4.20 | |||
| Wogonin | 2 | 95.8 | 4.12 | 99.8 | 3.18 | 102.9 | 4.12 | ||
| 10 | 99.7 | 4.51 | 104.3 | 2.58 | 101.3 | 2.51 | |||
| 20 | 99.1 | 3.79 | 97.4 | 3.10 | 99.6 | 3.15 | |||
Fig. 5 Extracted ion chromatograms of different positive samples
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