Rapid Detection of Five Estrogens Added Illegally to Dietary Supplements by Combining TLC with Raman Imaging Microscope
Abstract
:1. Introduction
2. Materials and Methods
2.1. Materials
2.2. Apparatus
2.3. Solutions Preparation
2.4. The TLC Method
2.5. The TLC-RIM Method
3. Results and Discussion
3.1. TLC Separation
3.2. The TLC-RIM Method
3.3. Correlation between Raman Spectra of Reference Powders and the Spectra by TLC-RIM
3.4. Analysis of Characteristic Peaks of Estrogens
3.5. Experiment of Simulated Positive Samples
3.6. Detection of the Limit of Detection
3.7. Detection of Real Samples
4. Conclusions
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Conflicts of Interest
Sample Availability
References
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Chemical Structure | Raman Shift (cm−1) of Estrogen Powders (Relative Intensity) | Raman Shift (cm−1) of Estrogen by TLC-RIM (Relative Intensity) | Assignments |
---|---|---|---|
E1 | 3068 (1.0) 2974, 2939 (1.8, 3.0) 2914, 2885 (2.0, 1.7) 1719 (0.8) 1590, 1615 (0.9, 1.0) 735, 723(1.4, 2.2) | 3058 (1.0) 2973, 2938 (2.0, 2.2) 2915, 2883 (1.2, 1.1) 1709 (0.5) 1589, 1612 (1.0, 1.1) 732, 721(1.0, 1.7) | ν=CH within phenyl rings νasCH3, νasCH2 νsCH3,νsCH2 νC=O νC=C γ=C-H within phenyl rings |
E2 | 3060 (1.0) 2964, 2939 (1.0, 2.0) 2913, 2858 (2.0, 1.0) 1619, 1612 (1.7, 1.4) 732, 725 (1.2, 0.6) | 3060 (1.0) 2960, 2936 (1.0, 1.6) 2911, 2853 (1.4, 1.3) 1622, 1609 (0.5, 0.4) 732, 722 (1.0, 0.4) | ν=CH within phenyl rings νasCH3, νasCH2 νsCH3,νsCH2 νC=C γ=C-H within phenyl rings |
E3 | 3060 (1.0) 2964, 2939 (1.0, 2.2) 2913, 2858 (1.3, 1.3) 1614 (0.7) 723, 709 (1.3, 0.7) | 3060 (1.0) 2960, 2936 (1.0, 1.6) 2911, 2853 (1.2, 1.2) 1613 (0.6) 732, 722 (1.2, 0.5) | ν=CH within phenyl rings νasCH3, νasCH2 νsCH3,νsCH2 νC=C γ=C-H within phenyl rings |
EE2 | 3056 (1.0) 2965, 2941 (1.4, 2.2) 2910, 2860 (1.6, 1.5) 2113, 2102 (1.4, 1.5) 1617, 1602 (0.7, 0.5) 735, 713 (1.0, 1.4) | 3063 (1.0) 2957, 2935 (1.5, 2.3) 2873, 2861 (1.8, 1.8) 2111 (1.7) 1615, 1601 (0.9, 0.6) 733, 716 (0.7, 1.2) | ν=CH within phenyl rings νasCH3, νasCH2 νsCH3,νsCH2 νC≡C νC=C γ=C-H within phenyl rings |
DES | 3058 (1.0) 2960, 2937 (0.3, 0.4) 2913, 2878 (0.3, 0.2) 1633 (1.2) 1608, 1600 (0.7, 0.1) 817 (0.8) | 3061 (1.0) 2960, 2930 (0.8, 0.7) 2902, 2870 (0.6, 0.6) 1629 (1.4) 1608, 1593 (1.2, 0.8) 821 (1.0) | ν=CH within phenyl rings νasCH3, νasCH2 νsCH3,νsCH2 νC=C symmetric vibration νC=C within phenyl rings γ=C-H within phenyl rings |
Drugs | The minimum Therapeutic Dosage in Oral Medications (mg/a Day) | Potentially Abused Dosages of Drugs in BDS (mg/a Single Dose) | The Possible Concentration of the Drug in Sample Solution (mg/mL) | LOD (mg/mL) |
---|---|---|---|---|
E1 | 1 | 1 | 10 | 0.4 |
E2 | 1 | 1 | 10 | 1.0 |
E3 | 1 | 1 | 10 | 0.8 |
EE2 | 0.02 | 0.02 | 0.2 | 0.2 |
DES | 0.25 | 0.25 | 2.5 | 0.2 |
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Liang, X.; Li, L.; Dong, Y.; Dong, W.; Cui, H.; Xia, C.; Xu, T.; Wang, C.; Zhang, J.; Liu, T.; et al. Rapid Detection of Five Estrogens Added Illegally to Dietary Supplements by Combining TLC with Raman Imaging Microscope. Molecules 2022, 27, 2650. https://doi.org/10.3390/molecules27092650
Liang X, Li L, Dong Y, Dong W, Cui H, Xia C, Xu T, Wang C, Zhang J, Liu T, et al. Rapid Detection of Five Estrogens Added Illegally to Dietary Supplements by Combining TLC with Raman Imaging Microscope. Molecules. 2022; 27(9):2650. https://doi.org/10.3390/molecules27092650
Chicago/Turabian StyleLiang, Xin, Li Li, Yan Dong, Wei Dong, Hongxia Cui, Chunhui Xia, Tao Xu, Chaozhong Wang, Jie Zhang, Tingting Liu, and et al. 2022. "Rapid Detection of Five Estrogens Added Illegally to Dietary Supplements by Combining TLC with Raman Imaging Microscope" Molecules 27, no. 9: 2650. https://doi.org/10.3390/molecules27092650