3-hydroxytanshinone IIA sodium sulfonate as well as preparation method and application thereof
A technology of hydroxysalvia and sodium sulfonate, applied in steroids, measuring devices, instruments, etc., can solve the problems of non-therapeutic related substances affecting product quality or product purity, etc.
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Embodiment 13
[0033] The separation and purification of embodiment 13-hydroxytanshinone II A sodium sulfonate
[0034]Get batch number and be 0908205 tanshinone IIA sodium sulfonate raw material 10g, dissolve with 20% methanol, adopt low-pressure reverse-phase column chromatography to separate, column chromatography filler is reverse-phase silica gel ODS-A (50 μ m, produced by YMC Company), and the packing quality used is 1000g , the packed column height is 1.2m, the mobile phase is 20% methanol solution, and the flow rate is 2 ml / s. Finally, pure methanol is used to flush the column. Two times of the column volume is a mobile phase fraction, and 7 groups of fractions are collected; The 2 streams were combined, and the above-mentioned low-pressure reversed-phase column chromatography was separated again, the mobile phase was 15% methanol solution, and the flow rate was 4 ml / s. Finally, pure methanol was used to flush the column, and 4 groups of fractions were collected; the second fraction w...
Embodiment 23
[0035] The structural identification of embodiment 23-hydroxytanshinone II A sodium sulfonate
[0036] Adopt Varian Inova-400 type nuclear magnetic resonance instrument (Varian company) to detect above-mentioned separation product, take TMS (tetramethylsilane) as internal standard substance, frequency 400MHz, solvent CD 3 OD, the detection data are as follows:
[0037] carbon number
Embodiment 33
[0038] Example 33-Hydroxytanshinone II A sodium sulfonate is used as a reference substance to determine related substances of tanshinone II A sodium sulfonate raw material
[0039] Use octadecylsilane bonded silica gel as filler, Diamonsil, C 18 (4.6×250mm, 5μm) chromatographic column, using methanol: 0.02mol / L disodium hydrogen phosphate solution as 65:35, dilute phosphoric acid to adjust the pH to 6.0 as the mobile phase; the detection wavelength is 271nm, and the flow rate is 1.0ml / min; The injection volume is 20 μl; take this product (see below for the batch number), which is equivalent to 2 mg of Tanshinone II A sodium sulfonate, put it in a 10 ml measuring bottle, add mobile phase to dissolve and dilute to the mark, shake well, and use it as the test solution; take 3 -Hydroxytanshinone II A sodium sulfonate reference substance 20mg is placed in a 100ml measuring bottle, diluted to the mark with mobile phase, shaken up, and used as a contrast solution; according to the ch...
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