Quality Assessment of Insamyangpye Decoction by Liquid Chromatography Tandem Mass Spectrometry Multiple Reaction Monitoring
Abstract
:1. Introduction
2. Materials and Methods
2.1. Plant Materials
2.2. Chemicals and Reagents
2.3. Preparation of ISYPD Extract
2.4. Preparation of Samples and Standard Solutions for the Quantitative Analysis
2.5. Instrument and Operating Conditions for Simultaneous Analysis of Compounds 1–10 in the ISYPD Sample
2.6. Validation of the LC–MS/MS MRM Method
3. Results and Discussion
3.1. Development of the LC–MS/MS MRM Method
3.2. MRM Transition of Each Marker Compound in the LC–MS/MS Simultaneous Analysis
3.3. Verification of the LC–MS/MS Method
3.4. Simultaneous Determination of Compounds 1–10 in the ISYPD Samples
4. Conclusions
Supplementary Materials
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Conflicts of Interest
References
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UPLC Conditions | MS (Mass Spectrometry) Conditions | ||||
---|---|---|---|---|---|
UPLC (Ultra performance liquid chromatography) system | Acquity UPLC H-Class | MS system | Xevo TQ-S micro | ||
Column | Acquity UPLC BEH C18 column (2.1 mm × 50 mm, 1.7 μm) | MS software | MassLynx (version 4.2) | ||
Column temp. | 30 °C | Ionization mode | ESI+ (Electrospray ionization positive)/ESI− (Electrospray ionization nagative) | ||
Sample temp. | 20 °C | Acquisition mode | MRM (multiple reaction monitoring) | ||
Injection volume | 2.0 μL | Capillary voltage | 3.3 V | ||
Flow rate | 0.3 mL/min | Cone gas flow | 80 L/h | ||
Mobile phase A | Distilled water with 0.1% TFA (trifluoroacetic acid) | Desolvation temp. | 300 °C | ||
Mobile phase B | Acetonitrile with 0.1% TFA | Desolvation gas flow | 300 L/h | ||
Gradient | Time (min) | A (%) | B (%) | Source temp. | 150 °C |
0.00 | 95 | 5 | |||
11.43 | 40 | 60 | |||
14.29 | 5 | 95 | |||
15.71 | 5 | 95 | |||
17.14 | 95 | 5 | |||
20.00 | 95 | 5 |
Markers | Ion Mode | Molecular Weight | MRM Transition | Cone Voltage (V) | Collision Energy (eV) | Retention Time (min) |
---|---|---|---|---|---|---|
1 | Positive | 568.18 | 569.21→244.99 | 16 | 18 | 2.40 |
2 | Positive | 457.16 | 480.14→347.01 | 96 | 26 | 2.84 |
3 | Negative | 550.17 | 549.15→118.94 | 76 | 48 | 4.16 |
4 | Positive | 580.18 | 581.18→152.94 | 18 | 44 | 4.83 |
5 | Positive | 594.19 | 595.21→286.98 | 6 | 20 | 6.23 |
6 | Positive | 1224.58 | 1225.66→485.23 | 14 | 46 | 6.57 |
7 | Positive | 1108.6 | 1109.7→162.94 | 28 | 44 | 7.57 |
8 | Positive | 822.4 | 823.46→453.2 | 18 | 20 | 8.48 |
9 | Positive | 780.47 | 781.51→437.2 | 14 | 16 | 9.09 |
10 | Positive | 432.21 | 433.22→346.01 | 26 | 24 | 9.25 |
Marker | Linear Range (μg/L) | Regression Equation a y = ax + b | r2 | LOD (μg/L) | LOQ (μg/L) |
---|---|---|---|---|---|
1 | 200.00–3200.00 | y = 16.61x − 30.28 | 0.9996 | 3.657 | 12.190 |
2 | 200.00–3200.00 | y = 2.34x + 31.68 | 0.9983 | 39.093 | 130.310 |
3 | 75.00–1200.00 | y = 1.06x − 14.60 | 0.9976 | 6.009 | 20.030 |
4 | 125.00–2000.00 | y = 18.62x + 59.88 | 0.9952 | 1.140 | 3.800 |
5 | 25.00–400.00 | y = 33.51x + 70.79 | 0.9996 | 2.151 | 7.170 |
6 | 7.50–120.00 | y = 3.45x + 2.65 | 0.9914 | 2.094 | 6.980 |
7 | 2.50–40.00 | y = 10.00x − 3.38 | 0.9989 | 0.002 | 0.005 |
8 | 75.00–1200.00 | y = 66.65x − 332.05 | 0.9997 | 6.939 | 23.130 |
9 | 7.50–120.00 | y = 23.00x + 3.17 | 0.9989 | 1.365 | 4.550 |
10 | 2.5.00–40.00 | y = 85.14x + 3.56 | 0.9986 | 0.123 | 0.410 |
Marker | Spiked Amount (μg/L) | Found Amount (μg/L) | Recovery (%) a | SD (Standard Deviation) | RSD (%) (Relative Standard Deviation (%)) |
---|---|---|---|---|---|
1 | 100.00 | 90.00 | 90.00 | 6.00 | 6.62 |
200.00 | 229.93 | 114.97 | 5.00 | 4.34 | |
400.00 | 417.20 | 104.30 | 2.30 | 2.25 | |
2 | 100.00 | 94.17 | 94.17 | 7.00 | 7.42 |
200.00 | 198.57 | 99.29 | 8.90 | 8.98 | |
400.00 | 428.97 | 107.24 | 6.10 | 5.67 | |
3 | 37.50 | 38.63 | 103.01 | 18.40 | 17.86 |
75.00 | 78.77 | 105.03 | 12.40 | 11.84 | |
150.00 | 165.60 | 110.40 | 4.20 | 3.78 | |
4 | 62.50 | 65.50 | 104.80 | 7.00 | 6.64 |
125.00 | 119.23 | 95.38 | 10.60 | 11.14 | |
250.00 | 263.23 | 105.29 | 8.40 | 7.97 | |
5 | 12.50 | 13.20 | 105.60 | 2.10 | 2.00 |
25.00 | 25.90 | 103.60 | 4.20 | 4.09 | |
50.00 | 53.53 | 107.06 | 6.50 | 6.04 | |
6 | 3.75 | 3.40 | 90.67 | 11.60 | 12.82 |
7.50 | 8.33 | 111.07 | 5.40 | 4.85 | |
15.00 | 16.27 | 108.47 | 8.40 | 7.78 | |
7 | 1.25 | 1.30 | 104.00 | 8.00 | 7.69 |
2.50 | 2.57 | 102.80 | 14.00 | 13.68 | |
5.00 | 4.67 | 93.40 | 17.90 | 19.21 | |
8 | 37.50 | 40.27 | 107.39 | 5.40 | 4.99 |
75.00 | 74.50 | 99.33 | 3.30 | 3.30 | |
150.00 | 152.80 | 101.87 | 1.00 | 1.02 | |
9 | 3.75 | 3.57 | 95.20 | 8.10 | 8.57 |
7.50 | 7.97 | 106.27 | 5.40 | 5.07 | |
15.00 | 14.07 | 93.80 | 11.70 | 12.52 | |
10 | 1.25 | 1.20 | 96.00 | 8.00 | 8.33 |
2.50 | 2.77 | 110.80 | 6.10 | 5.52 | |
5.00 | 5.43 | 108.60 | 11.40 | 10.47 |
Markers | Conc. (μg/L) | Intraday (n = 5) | Interday (n = 5) | ||||
---|---|---|---|---|---|---|---|
Observed Conc. (Concentration) (μg/L) | Precision (%) a | Accuracy (%) | Observed Conc. (μg/L) | Precision (%) | Accuracy (%) | ||
1 | 100.00 | 90.00 | 6.62 | 90.00 | 106.37 | 7.85 | 106.40 |
200.00 | 229.93 | 4.34 | 115.00 | 219.26 | 5.08 | 109.60 | |
400.00 | 417.20 | 2.25 | 104.30 | 371.90 | 11.46 | 93.00 | |
2 | 100.00 | 94.17 | 7.42 | 94.20 | 100.77 | 12.02 | 100.80 |
200.00 | 198.57 | 8.98 | 99.30 | 200.98 | 17.83 | 100.50 | |
400.00 | 428.97 | 5.67 | 107.20 | 392.52 | 13.05 | 98.10 | |
3 | 37.50 | 38.63 | 17.86 | 103.00 | 37.02 | 16.75 | 98.70 |
75.00 | 78.77 | 11.84 | 105.00 | 84.23 | 3.66 | 112.30 | |
150.00 | 165.60 | 3.78 | 110.40 | 151.03 | 15.01 | 100.70 | |
4 | 62.50 | 65.50 | 6.64 | 104.80 | 65.67 | 11.03 | 105.10 |
125.00 | 119.23 | 11.14 | 95.40 | 135.20 | 9.19 | 108.20 | |
250.00 | 263.23 | 7.97 | 105.30 | 262.77 | 13.83 | 105.10 | |
5 | 12.50 | 13.20 | 2.00 | 105.60 | 13.23 | 3.49 | 105.90 |
25.00 | 25.90 | 4.09 | 103.60 | 24.73 | 8.39 | 98.90 | |
50.00 | 53.53 | 6.04 | 107.10 | 48.17 | 16.48 | 96.30 | |
6 | 3.75 | 3.40 | 12.82 | 90.70 | 3.90 | 5.13 | 104.00 |
7.50 | 8.33 | 4.85 | 111.10 | 8.40 | 1.19 | 112.00 | |
15.00 | 16.27 | 7.78 | 108.40 | 14.67 | 14.05 | 97.80 | |
7 | 1.25 | 1.30 | 7.69 | 104.00 | 1.28 | 10.25 | 102.40 |
2.50 | 2.57 | 13.68 | 102.70 | 2.78 | 3.93 | 111.00 | |
5.00 | 4.67 | 19.21 | 93.30 | 4.96 | 15.15 | 99.10 | |
8 | 37.50 | 40.27 | 4.99 | 107.40 | 37.51 | 2.76 | 100.00 |
75.00 | 74.50 | 3.30 | 99.30 | 74.55 | 4.79 | 99.40 | |
150.00 | 152.80 | 1.02 | 101.90 | 148.97 | 5.63 | 99.30 | |
9 | 3.75 | 3.57 | 8.57 | 95.10 | 3.91 | 8.03 | 104.20 |
7.50 | 7.97 | 5.07 | 106.20 | 7.84 | 8.88 | 104.60 | |
15.00 | 14.07 | 12.52 | 93.80 | 15.08 | 8.92 | 100.50 | |
10 | 1.25 | 1.20 | 8.33 | 96.00 | 1.17 | 9.90 | 93.30 |
2.50 | 2.77 | 5.52 | 110.70 | 2.70 | 7.41 | 108.00 | |
5.00 | 5.43 | 10.47 | 108.70 | 5.33 | 8.86 | 106.70 |
Marker | Amount | ||
---|---|---|---|
Mean (mg/g) | SD | RSD (%) | |
1 | 7.47 | 0.33 | 4.35 |
2 | 6.12 | 0.25 | 4.05 |
3 | 1.72 | 0.09 | 5.09 |
4 | 3.86 | 0.18 | 4.76 |
5 | 1.08 | 0.12 | 10.71 |
6 | 0.37 | 0.04 | 11.09 |
7 | 0.09 | 0.01 | 11.84 |
8 | 2.69 | 0.02 | 0.60 |
9 | 0.36 | 0.01 | 1.79 |
10 | 0.10 | 0.00 | 1.15 |
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Seo, C.-S.; Lee, M.-Y. Quality Assessment of Insamyangpye Decoction by Liquid Chromatography Tandem Mass Spectrometry Multiple Reaction Monitoring. Processes 2021, 9, 831. https://doi.org/10.3390/pr9050831
Seo C-S, Lee M-Y. Quality Assessment of Insamyangpye Decoction by Liquid Chromatography Tandem Mass Spectrometry Multiple Reaction Monitoring. Processes. 2021; 9(5):831. https://doi.org/10.3390/pr9050831
Chicago/Turabian StyleSeo, Chang-Seob, and Mee-Young Lee. 2021. "Quality Assessment of Insamyangpye Decoction by Liquid Chromatography Tandem Mass Spectrometry Multiple Reaction Monitoring" Processes 9, no. 5: 831. https://doi.org/10.3390/pr9050831