Quantitative Comparative Analysis of the Bio-Active and Toxic Constituents of Leaves and Spikes of Schizonepeta tenuifolia at Different Harvesting Times
Abstract
:1. Introduction
2. Material and Methods
2.1. Plant Materials
2.2. Chemicals and Reagents
2.3. Preparation of Sample and Standard Solutions
2.4. GC-MS-SIM Analysis
2.5. Validation of the GC-MS-SIM Method
3. Results and Discussion
3.1. Identification of Chemical Components in the Volatile Oils
3.2. GC-MS-SIM Method Validation
3.3. Quantification of the Eight Compounds
4. Conclusions
Acknowledgements
References
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Samples No. | Harvesting time |
---|---|
L1 | Growing stage (August 25, 2009) |
L2 | Formation of spikes (September 2, 2009) |
L3, S3 | Formation of spikes (September 9, 2009) |
L4, S4 | Full bloom (September 16, 2009) |
L5, S5 | Full bloom (September 23, 2009) |
L6, S6 | Stage of fruitage (September 30, 2009) |
L7, S7 | Stage of fruitage (October 6, 2009) |
No. | Compound | RT/min | MW | Formula | Selected ion group | Internal standard |
---|---|---|---|---|---|---|
1 | 1-octen-3-ol | 7.66 | 128.21 | C8H16O | 43, 99, 128 | n-decane |
2 | 3-octanone | 7.93 | 129.21 | C8H14O | 72, 99, 128, | n-decane |
3 | β-myrcene | 8.12 | 136.23 | C10H16 | 27, 41, 93, 136 | n-decane |
4 | (−)-limonene | 9.8 | 136.24 | C10H16 | 69, 79, 136 | n-decane |
5 | (−)-menthone | 18.46 | 154.25 | C10H18O | 69, 112, 139, 154 | naphthalene |
6 | (+)-menthofuran | 19.35 | 150.22 | C10H14O | 79, 108, 150 | naphthalene |
7 | (+)-pulegone | 24.76 | 152.23 | C10H16O | 105, 112, 137, 152 | naphthalene |
8 | β-caryophyllene | 32.15 | 204.36 | C15H24 | 105, 120, 133, 204 | naphthalene |
Analyte | Calibration curve | r2 | Liner range (ng) | LOD (ng) | LOQ (ng) |
---|---|---|---|---|---|
1-octen-3-ol | y = 2.7312x − 7.3567 | 0.9998 | 5.7–227.7 | 1.0 | 2.8 |
3-octanone | y = 18.155x − 4.5699 | 0.9998 | 1.1–42.6 | 0.4 | 1.1 |
myrcene | y = 46.038x − 11.073 | 0.9998 | 2.0–80.1 | 0.8 | 2.0 |
(−)-limonene | y = 7.3369x + 51.41 | 0.9992 | 16.1–642.2 | 6.7 | 16.1 |
(−)-menthone | y = 0.3547x + 6.1814 | 0.9992 | 79.8–3191.7 | 2.5 | 8.3 |
(+)-menthofuran | y = 3.6063x − 0.4994 | 0.9996 | 0.5–19.5 | 0.2 | 0.5 |
(+)-pulegone | y = 0.1784x + 3.7122 | 0.9990 | 147.8–5911.0 | 12.5 | 41.7 |
β-caryophyllene | y = 0.5941x − 0.5272 | 0.9998 | 3.1–125.8 | 0.9 | 3.1 |
Analytes | Precision
| Repeatability (RSD, %, n = 6) | Stability (RSD, %, n = 6) | |
---|---|---|---|---|
Intra-day (n = 6) RSD (%) | Inter-day (n = 3) RSD (%) | |||
1-octen-3-ol | 0.46 | 0.32 | 1.51 | 0.65 |
3-octanone | 0.09 | 1.21 | 2.68 | 0.70 |
myrcene | 0.05 | 1.53 | 0.73 | 0.04 |
(−)-limonene | 0.13 | 2.28 | 2.37 | 0.09 |
(−)-menthone | 0.26 | 1.66 | 1.79 | 0.06 |
(+)-menthofuran | 0.42 | 0.29 | 2.24 | 1.44 |
(+)-pulegone | 0.16 | 1.87 | 1.92 | 0.40 |
β-caryophyllene | 0.18 | 1.33 | 2.00 | 1.22 |
Analytes | Original (μg) | Added (μg) | Found (μg) | Recovery (%) | RSD (%, n = 6) |
---|---|---|---|---|---|
1-octen-3-ol | 341.5 | 364.7 | 697.1 | 97.50 | 1.12 |
3-octanone | 56.2 | 62.0 | 120.5 | 103.79 | 1.25 |
myrcene | 110.4 | 117.4 | 231.4 | 103.11 | 1.73 |
(−)-limonene | 947.2 | 885.9 | 1852.2 | 102.16 | 2.56 |
(−)-menthone | 6026.4 | 5813.9 | 12157.4 | 105.45 | 1.50 |
(+)-menthofuran | 26.4 | 49.1 | 76.8 | 102.75 | 2.76 |
(+)-pulegone | 16862.6 | 16693.6 | 34031.6 | 102.85 | 2.47 |
β-caryophyllene | 319.5 | 340.7 | 666.1 | 101.75 | 1.28 |
Samples | Oil yield (g/g) | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 |
---|---|---|---|---|---|---|---|---|---|
L1 | 0.042 | 0.39 | 0.08 | 0.27 | 2.11 | 7.04 | 0.05 | 30.55 | 0.44 |
L2 | 0.044 | 0.65 | 0.10 | 0.28 | 2.07 | 7.90 | 0.05 | 32.35 | 0.44 |
L3 | 0.044 | 0.60 | 0.10 | 0.19 | 1.76 | 10.61 | 0.05 | 29.68 | 0.56 |
L4 | 0.036 | 0.51 | 0.07 | 0.17 | 1.40 | 9.39 | 0.02 | 24.02 | 0.37 |
L5 | 0.033 | 0.49 | 0.08 | 0.17 | 1.41 | 9.33 | 0.01 | 20.89 | 0.35 |
L6 | 0.036 | 0.49 | 0.09 | 0.18 | 1.53 | 12.49 | 0.01 | 18.25 | 0.34 |
L7 | 0.037 | 0.52 | 0.10 | 0.19 | 1.57 | 16.74 | 0.01 | 14.66 | 0.37 |
S3 | 0.050 | 0.34 | 0.07 | 0.22 | 2.61 | 0.95 | 0.02 | 41.86 | 0.55 |
S4 | 0.048 | 0.31 | 0.06 | 0.23 | 2.27 | 0.82 | 0.03 | 41.49 | 0.50 |
S5 | 0.052 | 0.34 | 0.07 | 0.29 | 2.57 | 0.78 | 0.12 | 45.41 | 0.35 |
S6 | 0.048 | 0.31 | 0.06 | 0.29 | 2.41 | 0.66 | 0.14 | 42.51 | 0.36 |
S7 | 0.048 | 0.30 | 0.07 | 0.33 | 2.54 | 0.54 | 0.15 | 42.84 | 0.34 |
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Yu, S.; Chen, Y.; Zhang, L.; Shan, M.; Tang, Y.; Ding, A. Quantitative Comparative Analysis of the Bio-Active and Toxic Constituents of Leaves and Spikes of Schizonepeta tenuifolia at Different Harvesting Times. Int. J. Mol. Sci. 2011, 12, 6635-6644. https://doi.org/10.3390/ijms12106635
Yu S, Chen Y, Zhang L, Shan M, Tang Y, Ding A. Quantitative Comparative Analysis of the Bio-Active and Toxic Constituents of Leaves and Spikes of Schizonepeta tenuifolia at Different Harvesting Times. International Journal of Molecular Sciences. 2011; 12(10):6635-6644. https://doi.org/10.3390/ijms12106635
Chicago/Turabian StyleYu, Sheng, Yiwen Chen, Li Zhang, Mingqiu Shan, Yuping Tang, and Anwei Ding. 2011. "Quantitative Comparative Analysis of the Bio-Active and Toxic Constituents of Leaves and Spikes of Schizonepeta tenuifolia at Different Harvesting Times" International Journal of Molecular Sciences 12, no. 10: 6635-6644. https://doi.org/10.3390/ijms12106635