Methods of Analysis of Steroids
An analytical method and compound technology, applied in the direction of analytical materials, material separation, measuring devices, etc., to achieve the effects of good stability, good applicability, and simple and convenient operation.
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Embodiment 1
[0042] Chromatographic conditions:
[0043] Chromatographic column: C18; 5μm; 4.6mm×250mm.
[0044] Mobile phase: acetonitrile: water = 43: 57 (volume ratio)
[0045] Injection volume: 50μl
[0046] Detection wavelength: 240nm
[0047] Flow rate: 1.0ml / min
[0048] Operation: Take an appropriate amount of sample, accurately weigh it, add acetonitrile to dissolve and quantitatively dilute to make a solution containing 0.4mg per 1ml, shake well, accurately measure 50μl and inject it into the liquid chromatograph, record the chromatogram, and obtain the normalization of the sample French liquid content.
[0049] Sample: the same batch number (060501) of halomethone and the intermediates involved in its synthesis, the liquid phase results are shown in the attached Figure 1-5 .
[0050] sample
Embodiment 2
[0052] Chromatographic conditions:
[0053] Chromatographic column: C18; 5um; 4.6mm×250mm.
[0054] Mobile phase: acetonitrile-water (4:6)
[0055] Injection volume: 50μl
[0056] Detection wavelength: 240nm
[0057] Flow rate: 1.0ml / min
[0058] Operation: Take an appropriate amount of 6 halomethasone samples, accurately weigh them, add acetonitrile to dissolve and quantitatively dilute to make a solution containing 0.8 mg per 1 ml, shake well, accurately measure 50 μl and inject it into a liquid chromatograph, and record the chromatogram; Normalized liquid phase content.
[0059] Sample 6 and sample 1 are the same batch of halomethone, the obtained liquid phase content: 98.96%, retention time (min): 17.732, see the attached HPLC figure Figure 6 .
Embodiment 3
[0061] Chromatographic conditions:
[0062] Chromatographic column: C18; 5μm; 4.6mm×250mm.
[0063] Mobile phase: acetonitrile-water (48:52)
[0064] Injection volume: 50μl
[0065] Detection wavelength: 245nm
[0066] Flow rate: 1.0ml / min
[0067] Operation: Take an appropriate amount of 7 halomethasone samples, accurately weigh them, add acetonitrile to dissolve and quantitatively dilute to make a solution containing 0.2mg per 1ml, shake well, accurately measure 50μl and inject it into the liquid chromatograph, and record the chromatogram; Normalized liquid phase content.
[0068] Sample 7 and sample 1 are the same batch of halomethone, the obtained liquid phase content: 99.06%, retention time (min): 9.107, the HPLC figure obtained is shown in the attached Figure 7 .
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