Table 3.
1H-NMR analysis of RYR dietary supplements: quantitative determination of monacolins (mg per capsule or tablet) 1 and list of other compounds identified.
| DS Number | Signal at 5.84 ppm 2 H6 | Signal at 5.56 ppm 2 H4 | Mean Intensity of Signals H6 and H4 |
Signal at 5.33 ppm 2 H1 | Signal at 4.60 ppm 2 H20 | Signal at 4.25 ppm 2 H22 | Compounds Identified Other than Monacolins 3,4 |
|---|---|---|---|---|---|---|---|
| 1 | 1.67 | 1.70 | 1.685 | 3.31 | 1.40 | 1.34 | SFA *, UFA, glycerol, glucose, monascin |
| 2 | 9.14 | 9.18 | 9.16 | 9.26 | 7.10 | SFA *, UFA, glycerol, glucose | |
| 3 | 3.07 | 3.07 | 3.07 | 2.39 | SFA *, UFA, carnitine *, vitamin B3 *, vitamin C * | ||
| 4 | 1.02 | 0.95 | 0.985 | 1.64 | 0.71 | SFA, UFA, glucose | |
| 5 | 2.47 | 2.53 | 2.50 | 11.3 | 2.15 | SFA *, UFA, glycerol, glucose, monascin | |
| 6 | 2.92 | 2.63 | 2.775 | 3.27 | 2.19 | SFA *, UFA, glucose, monascin | |
| 7 | 3.76 | 3.73 | 3.745 | SFA *, UFA, glucose, piperine * | |||
| 8 | 8.68 | 8.79 | 8.735 | 8.65 | 6.89 | 7.73 | SFA, UFA, glycerol, monascin |
| 9 | 5.14 | 5.21 | 5.125 | 8.03 | 4.55 | 4.55 | SFA *, UFA, glycerol, glucose, monascin |
| 10 | 2.10 | 2.04 | 2.07 | 8.67 | 1.22 | SFA, UFA, glycerol, glucose, monascin | |
| 11 | SFA, UFA, glycerol, glucose, monascin | ||||||
| 12 | SFA, UFA, glycerol, glucose, monascin | ||||||
| 13 | 23.9 | 23.9 | 23.9 | 21.9 | 23.9 | 23.2 | SFA *, UFA, glycerol, glucose |
| 14 | 3.45 | 3.28 | 3.365 | 10.8 | 2.26 | SFA, UFA, glycerol, glucose, monascin | |
| 15 | 11.9 | 12.3 | 12.1 | 9.85 | SFA *, UFA, glycerol, monascin | ||
| 16 | 0.31 | SFA *, UFA, glycerol, glucose, monascin, piperine * | |||||
| 17 | 1.47 | 1.51 | 1.49 | 4.06 | 1.28 | SFA, UFA, glycerol, monascin | |
| 18 | 8.84 | 8.19 | 8.515 | 6.68 | 7.04 | SFA *, UFA, glycerol, glucose, monascin | |
| 19 | 0.36 | 0.44 | 0.40 | SFA *, UFA, glycerol, glucose, monascin | |||
| 20 | 1.75 | 1.77 | 1.76 | 3.51 | 1.27 | 1.49 | SFA *, UFA, glycerol, glucose, monascin |
| 21 | 0.48 | 0.47 | 0.475 | SFA *, UFA, glycerol | |||
| 22 | 3.09 | 3.02 | 3.055 | 2.26 | SFA *, UFA, glycerol, glucose, monascin | ||
| 23 | 10.6 | 10.7 | 10.65 | 10.0 | 10.0 | 9.77 | SFA *, UFA, glycerol, glucose, monascin |
| 24 | 11.5 | 11.8 | 11.65 | 9.38 | 5.97 | SFA *, UFA, glucose, sorbitol * | |
| 25 | 10.0 | 9.72 | 9.87 | 5.97 | 7.26 | SFA, UFA, glycerol, monascin | |
| 26 | 4.51 | 4.54 | 4.525 | 3.88 | SFA *, UFA, glycerol, glucose, sorbitol | ||
| 27 | 4.13 | 3.84 | 3.985 | 2.97 | 2.90 | SFA, UFA, glycerol, glucose, monascin, chlorogenic acid * | |
| 28 | 1.64 | 1.75 | 1.695 | 1.05 | 1.31 | SFA *, UFA, glycerol, glucose | |
| 29 | SFA *, UFA, glycerol, glucose | ||||||
| 30 | 2.99 | 3.04 | 3.015 | 2.61 | 2.43 | SFA, UFA | |
| 31 | 1.21 | 1.28 | 1.245 | 2.16 | SFA *, UFA, glycerol, glucose, monascin, isopropanol |
1 The amounts of monacolins (mg per dosage unit) were calculated from the measured areas using the equation presented in the paragraph 3.4.2. 2 The resonances at 5.84, 5.56 ppm and 5.33 ppm are characteristic of all the monacolins bearing an hexahydronaphthalene ring but the 5.33 ppm signal does not characterize MJ and ML in lactone or in hydroxyl acid form; the resonances at 4.60 and 4.25 ppm are specific of all the monacolins in lactone form including dihydromonacolins. 3 SFA: saturated fatty acids; UFA: non-conjugated unsaturated fatty acids; monascin corresponds to monascin and other pigments with the same skeleton (see Table 2 and Figure 2 for the chemical structures of all these compounds). 4 The asterisk * means that the compound was mentioned on the label of the formulation.