Minoxidil Sulfate API 83701-22-8 White Crystalline Solid Against Hair Loss

Physical and chemical properties

Appearance and properties: white crystalline powder

Density: 1.52 g/cm3

Melting point: 272-274°C (dec.)(lit.)

Boiling point: 351.7 C at 760 mmHg

Flash: DHS 166.5 C

Refractive index: 1.724

Stable at normal temperatures and pressures.

Storage: Keep in a cool, dry location. Keep containers closed when not in use. Protect from light.

The synthetic methods

4-chloro-2, 6-diaminopyrimidine was obtained by cyclization and chlorination of methyl cyanoacetate, then oxidized with perbenzoic acid to obtain 6-amino-1, 2-dihydro-1-hydroxy-2-imino4-chloropyrimidine (C4H5CIN4O), and finally obtained minolidine by condensation with hexahydropyridine

Pharmacopoeia standard

Source (name), content (titer)

This product is 6- (1- piperidine) -2,4- pyrimidine diamine,3- oxide. C9H15N5O shall not be less than 99.0% as per dry product.

character

This product is white or white - like crystalline powder.

It is slightly soluble in ethanol, slightly soluble in chloroform or water, and extremely slightly soluble in acetone. Dissolved in glacial acetic acid.

To identify

(1) take this product, adding ethanol solvent and thinner each 1 ml contains about 6 mu g solution, according to the ultraviolet-visible spectrophotometry (2 2010 edition pharmacopoeia appendix Ⅳ A) determination, have the largest at the wavelength of 231 nm absorption.

(2) the infrared absorption spectrum of the product shall be consistent with the control spectrum (figure 608 of the infrared spectra collection of drugs).

check

Chlorinated compound

About 20 mg, take this product precision said, according to the oxygen flask combustion method (2 2010 edition pharmacopoeia appendix Ⅶ C) organic damage, with 10 ml of 0.1 mol/L sodium hydroxide solution as absorption liquid, after the course of burning, strong vibration wave for A few minutes, use A small amount of water to rinse the cork and platinum wire, lotion and people absorb liquid, remove the absorption liquid to 50 ml nessler tubes, according to the chloride method (2 2010 edition pharmacopoeia appendix Ⅷ A) inspection, and controlled liquid (with the test method of the operation, but does not contain in the filter paper test samples during burning, and join the standard sodium chloride solution of 4.0 ml), Not thicker (0.2%).

About the material

Take an appropriate amount of this product, accurately weigh it, dissolve it with mobile phase and dilute it to make a solution containing about 0.25mg per 1ml as the sample solution. An appropriate amount was precisely taken and diluted quantitatively with the mobile phase to make a solution containing about 2.5 g per 1ml as the control solution. According to high performance liquid chromatography (2 2010 edition pharmacopoeia appendix Ⅴ D) test. Using octadecylsilane bonded silica gel as filler; Methanol-water-glacial acetic acid (70:30:1) (containing 3.0g sodium dioctyl sulfonate per 1000ml, and adjusting the pH value to 3.0 with perchloric acid) was used as mobile phase. The detection wavelength is 240nm. The product and medroxyprogesterone acetate were dissolved in the mobile phase and diluted to make a mixture containing approximately 0.25mg each in 1ml. 10 solution l was taken and injected into the liquid chromatograph to record the chromatographic chart. The theoretical plate number was calculated according to minoxidil peak not less than 2000, and the separation degree of minoxidil peak and medroxyprogesterone acetate peak should be greater than 2.0. The control solution was precisely measured at 10 solution l and injected into the liquid chromatograph. The detection sensitivity was adjusted so that the peak height of the main component chromatographic peak was about 20% of the full range. The sample solution and the control solution were precisely measured at 10 solution l each and then injected into the liquid chromatograph. If there are impurity peaks in the chromatogram of the sample solution, the sum of the impurity peaks shall not be greater than the main peak area (1.0%) of the control solution.

Dry weight loss

Take this product, in 105 ℃ drying to constant weight, reduce weight loss may not be over 0.5% (2010 edition pharmacopoeia appendix Ⅷ L).

On ignition residue

Take this product is 1.0 g, in accordance with the inspection department ii (2010 edition pharmacopoeia appendix Ⅷ N), legacy residue may not be over 0.15%.

Heavy metal

Take on ignition residue of the residue left under, in accordance with the inspection (2 2010 edition pharmacopoeia appendix Ⅷ H second law), containing heavy metals shall not be twenty over one million.

Content determination

Take this product is about 0.15 g, precision said, add 50 ml glacial acetic acid, lukewarm dissolved, according to the potentiometric titration method (2 2010 edition pharmacopoeia appendix Ⅶ A), liquid with perchloric acid titration titration (0.1 mol/L), and the result of the titration correction by blank test. Each 1ml perchloric acid titrant (0.1mol/L) is equivalent to 20.93mg of C9H15N5O.