Graphene Assisted in the Analysis of Coumarins in Angelicae Pubescentis Radix by Dispersive Liquid–Liquid Microextraction Combined with 1H-qNMR
Abstract
:1. Introduction
2. Results and Discussion
2.1. Optimization of NMR Parameters
2.1.1. Choice of D1
2.1.2. Choice of NS
2.2. Optimization of DLLME-SFO Conditions
2.2.1. Choice of Extractant and Dispersant
2.2.2. Selection of Volume Ratio of Distilled Water to Test Sample Solution
2.2.3. Selection of Graphene Concentration in 1-Dodecyl Alcohol
2.2.4. Selection of Extractant Volume
2.2.5. Selection of Extractant Volume
2.2.6. Choice of Ionic Strength
2.2.7. Selection of Different Speed
2.2.8. Different Extraction Times
2.3. Methodology Validation
2.3.1. Linearity
2.3.2. Limit of Detection and Limit of Quantification
2.3.3. Precision
2.3.4. Stability and Repeatability
2.3.5. Recovery
2.4. Determination of the Samples
3. Materials and Methods
3.1. Reagent
3.2. Chemical
3.3. Method
3.3.1. Preparation of Sample Solution
3.3.2. Extraction Process of DLLME-SFO
3.3.3. NMR Acquisition and Processing Parameters
4. Conclusions
Author Contributions
Funding
Data Availability Statement
Conflicts of Interest
Sample Availability
References
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Detection Method | Extraction Method | ||||
---|---|---|---|---|---|
1H-qNMR | HPLC | DLLME-SFO | Other extraction methods | ||
Requirement on sample form | No specific requirements | Liquid | Volume of samples required | 1 mL | ≥10 mL |
Demand for reference substances | No | Yes | Need to stand layer | No | Yes |
Detection test | ≤5 min | >10 min | Extraction time | 20 min | >20 min |
Recycling of samples after measurement | Yes | No | Simultaneous separation and extraction | Yes | No |
Analyte | Linear Regression Equation | R2 | LOD (mg/mL) | LOQ (mg/mL) |
---|---|---|---|---|
OS | y = 0.0798x + 0.0008 | 0.9994 | 0.0660 | 0.2201 |
CO | y = 0.0822x + 0.0007 | 0.9994 | 0.0720 | 0.2401 |
IS | y = 0.0784x − 0.0011 | 0.9995 | 0.0620 | 0.2066 |
Analyte | Original Content (g) | Added Content (g) | Total Observed (g) | Recovery (%) | Average Recovery (%) | RSD (%) |
---|---|---|---|---|---|---|
OS | 0.0057 | 0.0057 | 0.0113 | 98.19 | 102.26 | 3.62 |
0.0117 | 104.46 | |||||
0.0117 | 106.12 | |||||
0.0112 | 97.37 | |||||
0.0117 | 105.13 | |||||
CO | 0.0085 | 0.0085 | 0.0170 | 100.07 | 99.89 | 3.86 |
0.0168 | 97.66 | |||||
0.0166 | 94.29 | |||||
0.0172 | 101.64 | |||||
0.0175 | 105.79 | |||||
IS | 0.0058 | 0.0057 | 0.0114 | 97.93 | 103.28 | 4.15 |
0.0121 | 109.33 | |||||
0.0118 | 103.68 | |||||
0.0115 | 99.11 | |||||
0.0119 | 106.34 |
Number | Content (g/g) | ||
---|---|---|---|
OS | CO | IS | |
1 | 0.0023 | 0.0040 | 0.0017 |
2 | 0.0016 | 0.0021 | - |
3 | 0.0024 | 0.0040 | - |
4 | 0.0003 | 0.0006 | 0.0007 |
5 | 0.0002 | 0.0010 | 0.0002 |
6 | 0.0026 | 0.0049 | 0.0030 |
7 | 0.0043 | 0.0061 | 0.0002 |
8 | 0.0042 | 0.0069 | 0.0007 |
9 | 0.0042 | 0.0069 | 0.0008 |
10 | 0.0020 | 0.0055 | 0.0015 |
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Feng, Y.; Li, Q.; Qiu, D.; Li, G. Graphene Assisted in the Analysis of Coumarins in Angelicae Pubescentis Radix by Dispersive Liquid–Liquid Microextraction Combined with 1H-qNMR. Molecules 2021, 26, 2416. https://doi.org/10.3390/molecules26092416
Feng Y, Li Q, Qiu D, Li G. Graphene Assisted in the Analysis of Coumarins in Angelicae Pubescentis Radix by Dispersive Liquid–Liquid Microextraction Combined with 1H-qNMR. Molecules. 2021; 26(9):2416. https://doi.org/10.3390/molecules26092416
Chicago/Turabian StyleFeng, Yanmei, Qian Li, Daiyu Qiu, and Guichen Li. 2021. "Graphene Assisted in the Analysis of Coumarins in Angelicae Pubescentis Radix by Dispersive Liquid–Liquid Microextraction Combined with 1H-qNMR" Molecules 26, no. 9: 2416. https://doi.org/10.3390/molecules26092416