Integrated LC-MS/MS Analytical Systems and Physical Inspection for the Analysis of a Botanical Herbal Preparation
Abstract
:1. Introduction
2. Results and Discussion
2.1. Method Development
MW a | Ion Mode | RT b | CE c | Q1 Mass d | Q3 Mass d | |
---|---|---|---|---|---|---|
Astragalus membranaceus | ||||||
Astragaloside I | 868.4 | + | 5.8 | −19 | 869.3 [M + H]+ | 143.0 |
Astragaloside IV | 784.9 | + | 6.4 | −21 | 785.3 [M + H]+ | 143.3 |
Formononetin | 268.3 | + | 5.2 | −42 | 269.1 [M + H]+ | 197.0 |
Paeonia lactiflora | ||||||
Paeoniflorin | 480.2 | + | 3.6 | −26 | 498.3 [M + NH4]+ | 179.1 |
Zingiber officinale | ||||||
Gingerol | 294.3 | + | 5.2 | −25 | 312.0 [M + NH4]+ | 137.2 |
Cinnamomum cassia | ||||||
Cinnamic acid | 148.1 | − | 3.4 | 15 | 147.1 [M − H]− | 103.0 |
Carvedilol (IS) | 406.4 | + | 4.9 | −35 | 407.1 [M + H]+ | 100.1 |
Tolbutamide (IS) | 270.3 | − | 4.4 | 20 | 269.0 [M − H]− | 170.0 |
2.2. Method Validation
Nominal Concentration (ng/mL) | Intra-Day | Inter-Day | ||||
---|---|---|---|---|---|---|
Observed Concentration (ng/mL) | Accuracy (%) | Precision (%) | Observed Concentration (ng/mL) | Accuracy (%) | Precision (%) | |
Astragaloside I | ||||||
25 | 25.21 ± 1.49 | 0.86 | 5.90 | 23.83 ± 0.85 | −4.68 | 3.55 |
50 | 47.68 ± 3.93 | −4.64 | 8.24 | 48.78 ± 1.73 | −2.44 | 3.56 |
250 | 259.48 ± 5.70 | 3.79 | 2.20 | 237.78 ± 5.93 | −4.89 | 2.49 |
500 | 488.38 ±15.04 | −2.32 | 3.08 | 512.51 ± 13.76 | 2.50 | 2.69 |
1000 | 987.19 ± 9.88 | −1.28 | 1.00 | 983.27 ± 22.24 | −1.67 | 2.26 |
Astragaloside IV | ||||||
10 | 9.23 ± 0.46 | −7.72 | 4.98 | 9.82 ± 1.34 | −1.84 | 13.61 |
50 | 23.64 ± 1.44 | 5.43 | 6.08 | 49.21 ± 3.29 | −1.58 | 6.68 |
250 | 50.21 ± 1.14 | 0.41 | 2.26 | 250.03 ± 7.69 | 0.01 | 3.08 |
500 | 246.48 ± 8.80 | −1.41 | 3.57 | 515.21 ± 5.45 | 3.04 | 1.06 |
1000 | 517.22 ± 6.27 | 3.44 | 1.21 | 997.18 ± 0.68 | −0.28 | 0.07 |
Formononetin | ||||||
25 | 22.81 ± 1.33 | −8.75 | 5.82 | 22.08 ± 0.47 | −11.67 | 2.12 |
50 | 46.01 ± 1.93 | −7.98 | 4.19 | 46.77 ± 2.34 | −6.46 | 5.01 |
250 | 253.44 ± 10.43 | 1.38 | 4.11 | 254.42 ± 5.85 | 1.77 | 2.30 |
500 | 506.04 ± 10.04 | 1.21 | 1.98 | 509.04 ± 15.79 | 1.81 | 3.10 |
1000 | 995.55 ± 2.29 | −0.44 | 0.23 | 994.74 ± 6.45 | −0.53 | 0.65 |
Cinnamic acid | ||||||
25 | 27.69 ± 1.95 | 10.74 | 7.05 | 26.32 ± 1.53 | 5.29 | 5.83 |
50 | 53.33 ± 1.62 | 6.65 | 3.04 | 49.83 ± 3.40 | −0.33 | 6.82 |
250 | 243.41 ± 5.31 | −2.64 | 2.18 | 236.01 ± 11.10 | −5.60 | 4.70 |
500 | 497.55 ± 10.83 | −0.49 | 2.18 | 487.97 ± 23.74 | −2.41 | 4.87 |
1000 | 1001.63 ± 5.97 | 0.16 | 0.60 | 997.47 ± 8.11 | −0.25 | 0.81 |
Paeoniflorin | ||||||
25 | 24.99 ± 1.55 | −0.04 | 6.21 | 24.50 ± 3.31 | −2.01 | 13.50 |
50 | 49.44 ± 3.38 | −1.13 | 6.83 | 51.09 ± 4.00 | 2.17 | 7.84 |
250 | 257.68 ± 16.41 | 3.07 | 6.37 | 245.60 ± 10.78 | −1.76 | 4.39 |
500 | 501.05 ± 7.91 | 0.21 | 1.58 | 505.76 ± 1.82 | 1.15 | 0.36 |
1000 | 993.47 ± 9.92 | −0.65 | 1.00 | 998.49 ± 0.90 | −0.15 | 0.09 |
Gingerol | ||||||
10 | 9.58 ± 0.84 | −4.25 | 8.82 | 9.26 ± 0.47 | 7.38 | 5.10 |
50 | 49.13 ± 1.79 | −1.74 | 3.65 | 50.31 ± 2.26 | 0.61 | 4.49 |
250 | 251.93 ± 2.66 | 0.77 | 1.05 | 251.84 ± 7.15 | 0.73 | 2.84 |
500 | 500.08 ± 7.34 | 0.02 | 1.47 | 497.17 ± 8.01 | −0.57 | 1.61 |
1000 | 999.65 ± 3.05 | −0.04 | 0.31 | 1000.92 ± 2.27 | 0.09 | 0.23 |
2.3. Application to the HGW Samples
Components | EX | A | B | C | D | E |
---|---|---|---|---|---|---|
Astragaloside I | 0.46 ± 0.024 | 0.31 ± 0.007 | 0.52 ± 0.005 | 0.81 ± 0.004 | 0.39 ± 0.006 | 0.36 ± 0.001 |
Astragaloside IV | 0.09 ± 0.002 | 0.12± 0.005 | 0.16 ± 0.003 | 0.10 ± 0.003 | 0.08± 0.002 | 0.07 ± 0.001 |
Formononetin | 0.83 ± 0.021 | 0.31 ± 0.004 | 0.68 ± 0.010 | 0.46 ± 0.006 | 0.54 ± 0.006 | 0.34 ± 0.002 |
Cinnamic acid | 0.24 ± 0.010 | 0.32 ± 0.009 | 0.34 ± 0.005 | 0.19 ± 0.006 | 0.31 ± 0.007 | 0.17 ± 0.004 |
Paeoniflorin | 4.15 ± 0.044 | 2.26 ± 0.013 | 3.72 ± 0.003 | 2.09 ± 0.047 | 2.97 ± 0.002 | 1.67 ± 0.016 |
Gingerol | 0.08 ± 0.003 | 0.91 ± 0.006 | 0.25 ± 0.007 | 0.36 ± 0.010 | 0.30 ± 0.007 | 0.80 ± 0.001 |
2.4. Physical Examination of the Pharmaceutical Additives
2.4.1. Scanning Electron Microscopy
2.4.2. Light Microscopy Images of Congo red and Iodine-KI Stained Samples
2.4.3. Solubility and Swelling Experiment
Sample Brand | 55 °C | 65 °C | 75 °C | 85 °C | 95 °C |
---|---|---|---|---|---|
A | 38.73 ± 2.77 | 38.84 ± 0.72 | 40.82 ± 3.60 | 42.59 ± 0.19 | 45.74 ± 2.07 |
B | 45.95 ± 4.84 | 47.78 ± 2.61 | 46.18 ±0.62 | 50.13 ± 0.94 | 52.97 ± 2.93 |
C | 40.97 ± 2.58 | 42.19 ± 1.47 | 43.62 ± 1.31 | 42.76 ± 1.32 | 48.81 ± 3.95 |
D | 33.67 ± 2.31 | 35.20 ± 0.97 | 39.95 ± 2.94 | 38.77 ± 1.68 | 40.64 ± 3.89 |
E | 39.51 ± 0.19 | 41.33 ± 3.22 | 42.51 ± 2.85 | 41.63 ± 5.62 | 45.49 ± 1.56 |
Sample Brand | 55 °C | 65 °C | 75 °C | 85 °C | 95 °C |
---|---|---|---|---|---|
A | 4.99 ± 0.71 | 6.26 ± 0.31 | 6.22 ± 0.82 | 7.41 ± 0.28 | 6.86 ± 1.14 |
B | 5.96 ± 1.64 | 7.44 ± 1.38 | 8.83 ± 0.21 | 8.79 ± 1.44 | 6.69 ± 1.19 |
C | 6.43 ± 0.57 | 6.15 ± 1.09 | 8.93 ± 0.35 | 7.45 ± 1.99 | 4.74 ± 0.71 |
D | 4.78 ± 0.31 | 5.37 ± 0.71 | 5.42 ± 1.58 | 5.59 ± 0.53 | 7.71 ± 1.54 |
E | 4.04 ± 0.41 | 4.57 ± 0.89 | 5.81 ± 0.43 | 5.25 ± 0.85 | 6.60 ± 0.60 |
2.4.4. Crude Fiber Content
3. Experimental Section
3.1. Reagents and Materials
3.2. Preparation of Herbal Extraction
3.3. UPLC-ESI-MS/MS System and Experimental Condition
3.4. Preparation of the Sample
3.5. Preparation of the Samples
3.6. Physical Examination of Additives for Raw Herbal Powder
3.6.1. Scanning Electron Microscope
3.6.2. Light Microscopy Images of Congo Red and Iodine-KI Stained Samples
3.6.3. Solubility and Swelling Experiments
3.6.4. Crude Fiber Analysis
4. Conclusions
Acknowledgments
Author Contributions
Conflicts of Interest
References
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Lai, K.-M.; Cheng, Y.-Y.; Tsai, T.-H. Integrated LC-MS/MS Analytical Systems and Physical Inspection for the Analysis of a Botanical Herbal Preparation. Molecules 2015, 20, 10641-10656. https://doi.org/10.3390/molecules200610641
Lai K-M, Cheng Y-Y, Tsai T-H. Integrated LC-MS/MS Analytical Systems and Physical Inspection for the Analysis of a Botanical Herbal Preparation. Molecules. 2015; 20(6):10641-10656. https://doi.org/10.3390/molecules200610641
Chicago/Turabian StyleLai, Kuan-Ming, Yung-Yi Cheng, and Tung-Hu Tsai. 2015. "Integrated LC-MS/MS Analytical Systems and Physical Inspection for the Analysis of a Botanical Herbal Preparation" Molecules 20, no. 6: 10641-10656. https://doi.org/10.3390/molecules200610641