Simultaneous Qualitative and Quantitative Analysis of Multiple Chemical Constituents in YiQiFuMai Injection by Ultra-Fast Liquid Chromatography Coupled with Ion Trap Time-of-Flight Mass Spectrometry
Abstract
:1. Introduction
2. Results and Discussion
2.1. Optimization of Chromatographic Conditions
2.2. Identification of Chemical Constituents in YQFM
2.2.1. Identification of Compounds in O. japonicus
2.2.2. Identification of Compounds in P. ginseng
2.2.3. Identification of Compounds in S. chinensis
2.3. Quantitative Analysis of 21 Compounds in YQFM by UFLC-IT-TOF/MS
2.3.1. Method Validation
2.3.2. Method Application for Quantification of 10 Batches of YQFM
3. Materials and Methods
3.1. Chemicals and Materials
3.2. Standard Solutions and Sample Preparation
3.2.1. Standard Solutions Preparation
3.2.2. Sample Solution Preparation
3.2.2.1. Sample Solutions for Qualitative Analysis
3.2.2.2. Sample Solutions for Quantitative Analysis
3.3. UFLC-IT-TOF/MS Analysis Conditions
3.3.1. Qualitative Analysis Conditions
3.3.2. Quantitative Analysis Conditions
3.4. Method Validation
3.4.1. Specificity
3.4.2. Linear Range and Sensitivity
3.4.3. Precision, Stability, Reproducibility and Accuracy
3.5. Application to Analysis of Samples of YQFM
4. Conclusions
Supplementary Materials
Acknowledgments
Author Contributions
Conflicts of Interest
Abbreviations
YQFM | YiQiFuMai injection |
UFLC-IT-TOF/MS | Ultra-fast liquid chromatography coupled with ion trap time-of-flight mass spectrometry |
BPC | Base peak chromatogram |
SPE | Solid phase extraction |
TCM | Traditional Chinese Medicine |
SMS | Sheng-mai San |
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Analyte | Y1 | Y2 | Y3 | Y4 | Y5 | Y6 | Y7 | Y8 | Y9 | Y10 |
---|---|---|---|---|---|---|---|---|---|---|
Peak 25 | 10.03 ± 0.12 | 10.54 ± 0.22 | 9.26 ± 0.40 | 8.35 ± 0.26 | 9.31 ± 0.33 | 9.22 ± 0.10 | 8.94 ± 0.20 | 9.81 ± 0.12 | 9.58 ± 0.21 | 9.93 ± 0.17 |
Peak 28 | 340.79 ± 9.34 | 338.47 ± 5.92 | 335.26 ± 14.29 | 291.53 ± 1.52 | 309.36 ± 2.44 | 316.55 ± 5.08 | 300.84 ± 4.62 | 316.60 ± 6.92 | 309.69 ± 2.47 | 337.38 ± 0.42 |
Peak 32 | 20.53 ± 0.74 | 20.16 ± 0.12 | 18.82 ± 0.10 | 14.27 ± 0.02 | 18.44 ± 0.86 | 18.80 ± 0.26 | 17.84 ± 0.20 | 20.36 ± 0.94 | 18.34 ± 0.78 | 21.90 ± 0.02 |
Re | 239.22 ± 4.41 | 252.46 ± 2.39 | 260.48 ± 1.60 | 258.82 ± 3.84 | 269.16 ± 1.87 | 269.12 ± 5.50 | 264.25 ± 3.79 | 260.87 ± 0.35 | 260.10 ± 3.79 | 259.90 ± 3.60 |
Rg1 | 1655.22 ± 71.14 | 1718.39 ± 70.12 | 1763.12 ± 59.12 | 1726.97 ± 10.05 | 1822.21 ± 2.40 | 1798.42 ± 35.13 | 1744.87 ± 17.27 | 1596.24 ± 10.16 | 1646.69 ± 17.24 | 1880.85 ± 6.02 |
Rf | 681.40 ± 15.78 | 608.42 ± 3.51 | 603.54 ± 16.76 | 751.55 ± 8.44 | 792.20 ± 38.74 | 810.92 ± 22.34 | 734.34 ± 34.89 | 809.52 ± 32.91 | 734.60 ± 33.41 | 878.60 ± 23.79 |
Rb1 | 1862.88 ± 34.38 | 1712.90 ± 25.32 | 1410.29 ± 65.97 | 1913.08 ± 93.66 | 2111.27 ± 80.02 | 2049.96 ± 3.82 | 1929.42 ± 71.45 | 2071.68 ± 29.32 | 2077.31 ± 77.55 | 2352.52 ± 37.43 |
S-Rg2 | 20.45 ± 0.31 | 19.60 ± 0.29 | 18.65 ± 0.16 | 20.83 ± 0.06 | 20.30 ± 0.28 | 20.53 ± 0.10 | 21.30 ± 0.85 | 20.49 ± 0.22 | 20.17 ± 0.19 | 20.65 ± 0.11 |
Ro | 1538.77 ± 69.92 | 1474.66 ± 4.35 | 1313.99 ± 40.31 | 1615.63 ± 40.01 | 1573.38 ± 18.22 | 1632.99 ± 35.10 | 1606.87 ± 25.73 | 1657.41 ± 57.58 | 1623.26 ± 15.37 | 1673.61 ± 43.11 |
Rh1 | 473.68 ± 10.32 | 446.74 ± 2.02 | 388.87 ± 0.19 | 452.80 ± 3.69 | 427.09 ± 2.40 | 430.71 ± 9.74 | 429.85 ± 18.48 | 434.27 ± 4.07 | 417.29 ± 2.54 | 435.27 ± 1.74 |
Rc | 84.83 ± 2.88 | 82.08 ± 2.00 | 80.59 ± 2.03 | 75.90 ± 0.13 | 79.84 ± 2.22 | 79.33 ± 0.53 | 78.03 ± 2.13 | 81.99 ± 3.66 | 76.47 ± 0.82 | 80.25 ± 1.38 |
Rb2 | 477.20 ± 2.00 | 459.21 ± 1.74 | 419.09 ± 9.67 | 478.33 ± 3.28 | 495.10 ± 3.62 | 509.51 ± 21.34 | 483.88 ± 13.24 | 516.15 ± 15.09 | 483.72 ± 7.12 | 521.33 ± 3.29 |
Rb3 | 98.25 ± 4.30 | 98.91 ± 0.80 | 89.71 ± 3.43 | 97.38 ± 0.58 | 103.03 ± 3.93 | 107.85 ± 0.86 | 101.33 ± 2.40 | 103.45 ± 4.03 | 97.51 ± 1.00 | 106.48 ± 2.91 |
Rd | 672.80 ± 2.28 | 634.78 ± 3.03 | 601.17 ± 6.81 | 750.13 ± 29.17 | 760.54 ± 5.51 | 766.45 ± 1.01 | 727.08 ± 20.25 | 732.32 ± 23.51 | 728.89 ± 14.60 | 777.63 ± 6.88 |
F2 | 2.10 ± 0.06 | 2.12 ± 0.07 | 2.19 ± 0.05 | 2.55 ± 0.07 | 2.68 ± 0.01 | 2.78 ± 0.02 | 2.46 ± 0.07 | 2.62 ± 0.11 | 2.52 ± 0.08 | 2.77 ± 0.02 |
R-Rg3 | 143.24 ± 3.05 | 125.54 ± 1.43 | 101.18 ± 4.62 | 142.83 ± 4.49 | 143.42 ± 2.03 | 144.29 ± 3.34 | 143.62 ± 2.96 | 155.16 ± 2.29 | 144.93 ± 1.40 | 151.46 ± 1.20 |
Rk1 | 84.54 ± 1.54 | 72.62 ± 1.72 | 59.09 ± 3.16 | 86.94 ± 1.27 | 88.67 ± 1.98 | 88.81 ± 0.71 | 86.57 ± 1.10 | 94.12 ± 0.75 | 89.53 ± 4.26 | 94.05 ± 3.23 |
R-Rh2 | 0.94 ± 0.04 | 0.64 ± 0.02 | 0.71 ± 0.02 | 0.87 ± 0.01 | 0.98 ± 0.02 | 0.99 ± 0.01 | 0.92 ± 0.04 | 1.06 ± 0.04 | 1.04 ± 0.03 | 0.93 ± 0.02 |
Schizandrol A | 129.08 ± 1.90 | 132.32 ± 1.70 | 123.19 ± 4.82 | 153.32 ± 2.64 | 155.45 ± 2.93 | 150.29 ± 2.66 | 142.81 ± 3.76 | 137.67 ± 4.66 | 142.85 ± 1.92 | 147.75 ± 1.46 |
Gomisin D | 4.39 ± 0.13 | 4.90 ± 0.14 | 4.98 ± 0.02 | 5.56 ± 0.27 | 6.03 ± 0.29 | 5.67 ± 0.05 | 5.84 ± 0.04 | 5.77 ± 0.21 | 6.10 ± 0.04 | 5.69 ± 0.14 |
Schizandrol B | 5.83 ± 0.20 | 6.52 ± 0.28 | 6.00 ± 0.25 | 7.03 ± 0.18 | 6.37 ± 0.10 | 6.82 ± 0.21 | 6.68 ± 0.32 | 6.55 ± 0.18 | 6.42 ± 0.22 | 6.31 ± 0.10 |
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Liu, C.; Ju, A.; Zhou, D.; Li, D.; Kou, J.; Yu, B.; Qi, J. Simultaneous Qualitative and Quantitative Analysis of Multiple Chemical Constituents in YiQiFuMai Injection by Ultra-Fast Liquid Chromatography Coupled with Ion Trap Time-of-Flight Mass Spectrometry. Molecules 2016, 21, 640. https://doi.org/10.3390/molecules21050640
Liu C, Ju A, Zhou D, Li D, Kou J, Yu B, Qi J. Simultaneous Qualitative and Quantitative Analysis of Multiple Chemical Constituents in YiQiFuMai Injection by Ultra-Fast Liquid Chromatography Coupled with Ion Trap Time-of-Flight Mass Spectrometry. Molecules. 2016; 21(5):640. https://doi.org/10.3390/molecules21050640
Chicago/Turabian StyleLiu, Chunhua, Aichun Ju, Dazheng Zhou, Dekun Li, Junping Kou, Boyang Yu, and Jin Qi. 2016. "Simultaneous Qualitative and Quantitative Analysis of Multiple Chemical Constituents in YiQiFuMai Injection by Ultra-Fast Liquid Chromatography Coupled with Ion Trap Time-of-Flight Mass Spectrometry" Molecules 21, no. 5: 640. https://doi.org/10.3390/molecules21050640