포비돈 K30

포비돈 K30

Pyrrolidone and acetylene were pressurized to form vinylpyrrolidone monomer. The 1-vinyl-2-pyrrolidone homopolymer was obtained by catalyst polymerization with an average molecular weight of 3.8×104. The molecular formula is (C6H9NO) n, where n represents the average number of 1-vinyl-2-pyrrolidone chains. According to the anhydrous matter, the nitrogen (N) content should be 11.5% ~ 12.8%.

【 Properties 】 This product is white to milky white powder; No odor or slightly extra odor.

This product is easily soluble in water, methanol or ethanol, very slightly soluble in acetone, insoluble in ether.

[Identification] (1) Take 2ml aqueous solution of this product (l→50), add 2ml of lmol/L hydrochloric acid solution and a few drops of potassium dichromate test solution to generate orange-yellow precipitate.

(2) Take 3ml aqueous solution of this product (l→50), add about 15mg cobalt nitrate and about 75mg ammonium thiocyanate, stir, drop dilute hydrochloric acid to make it acidic, that is, generate light blue precipitate.

(3) Take 3ml of aqueous solution of this product (l→50), add 1 ~ 2 drops of iodine test solution, that is, generate brownish-red precipitate, stir, dissolve into brownish-red solution.

(4) Take an appropriate amount of this product, dry at 105°C for 6 hours, according to the law, the infrared light absorption spectrum of this product should be consistent with that of the control product (general rule 0402).

[Check] Acidity Take 1.0g of this product, add 20ml of water to dissolve, check according to law (general rule 0631), pH value should be 3.0 ~ 5.0.

The clarity and color of the solution take 1.0g of this product, add 20ml of water to dissolve, the solution should be clear and colorless, such as turbidity, and No. 1 turbidity standard liquid (general rule 0902) compared, not thicker; Such as color, with yellow No. 1 or brown red No. 2 standard colorimetric solution (general 0901 first method) compared, not deeper.

Take 1.00g of this product (calculated as anhydrous matter), weigh it accurately, put it in a 100ml measuring bottle, add appropriate amount of water to dissolve it, and dilute it to the scale. After placing it in a constant temperature water bath of 25°C±0.2°C for 1 hour, check it according to law (the second method of general rule 0633), the relative viscosity ηr is measured, and calculate K value according to the following formula, which should be 27.0 ~ 32.0.

Take 1.0g of aldehyde, place it in a 100ml bottle, add phosphate buffer (take 1.74g potassium dihydrogen phosphate, dissolve it with 80ml water, adjust the pH value to 9.0 with 1mol/L potassium hydroxide solution, and then dilute it with water to 100ml, then get it), dissolve and dilute it to the scale, shake well, plug it, and place it in a constant temperature water bath at 60°C for 1 hour. Let cool and use as test solution. Take another acetaldehyde ammonia trimer 0.140g, put it in 200ml measuring bottle, dissolve it with water and dilute it to the scale, shake well, measure 1ml precisely, put it in 100ml measuring bottle, dilute it with phosphate buffer to the scale, shake well, and use it as a control solution. Accurately measure 0.5ml of the test solution, place it in a colorimetric dish, add 2.5ml phosphate buffer in turn, and then add nicotinamide adenine dinucleotide solution (take appropriate amount of β-nicotinamide adenine dinucleotide, put it in a glass bottle, dissolve and dilute it with phosphate buffer to make a solution containing 4mg per 1ml, store it at 4°C and become stable within 4 weeks) 0.2ml, cap it, and seal it. Mix well and place in a 22°C±2°C water bath for 2 ~ 3 minutes. With water as the reference, the absorbance was measured at the wavelength of 340nm by UV-visible spectrophotometry (general rule 0401). Then add aldehyde dehydrogenase solution in the same colorimetric dish (take an appropriate amount of low pressure lyophilized powder aldehyde dehydrogenase, put it in a glass bottle, dissolve and dilute it with water to make a solution containing 7U per 1ml, store it at 4°C and be stable within 8 hours) 0.05ml, cover it, mix it well, and place it in a water bath at 22°C±2C for 5 minutes. The absorbance is measured at the wavelength of 340nm with water as the reference. Take blank solution (water) and reference solution in the same way. Calculate the aldehyde content according to the following formula, calculated by acetaldehyde, not more than 0.05%.

Where At1 is the absorbance of the test product solution before adding aldehyde dehydrogenase;

At2 is the absorbance of the test product solution after adding aldehyde dehydrogenase.

As1 is the absorbance of reference solution before adding aldehyde dehydrogenase.

As2 is the absorbance of the control solution after adding aldehyde dehydrogenase.

Ab1 is the absorbance of blank solution before adding aldehyde dehydrogenase.

Ab2 is the absorbance of blank liquid after adding aldehyde dehydrogenase.

C is the concentration of the reference solution, mg/ml (the coefficient of conversion of acetaldehyde ammonia trimer to acetaldehyde is 0.72);

m is the sample amount (calculated as anhydrous matter), g.

Take about 0.25g of N-vinylpyrrolidone, weigh it accurately, put it in a 10ml bottle, dissolve it with mobile phase, dilute it to the scale, shake well, and use it as the test solution. Take an appropriate amount of N-vinylpyrrolidone as a reference product, weigh it accurately, dissolve and dilute it with methanol to make a solution containing about 5μg per 1ml, measure 5ml accurately, place it in a 100ml measuring bottle, dilute it with mobile phase to the scale, and shake well as a reference solution. A solution containing 1μg of N-vinylpyrrolidone and 50μg of vinyl acetate per 1ml was prepared by adding an appropriate amount of methanol to dissolve the N-vinylpyrrolidone reference product and vinyl acetate as the system suitability test solution. The method was determined by high performance liquid chromatography (general rule 0512) with octadecylsilane bonded silica gel as filler and acetonitrile-water (10:90) as mobile phase. The detection wavelength was 235nm. The system suitability test solution of 20μl was injected into the liquid chromatograph. The separation degree of N-vinylpyrrolidone peak and vinyl acetate peak should be greater than 6.0, and the separation degree of N-vinylpyrrolidone and adjacent chromatographic peaks in the test solution should meet the requirements. The test solution and the control solution were accurately measured to 20μl each, injected into the liquid chromatograph, recorded the chromatogram, calculated by the peak area according to the external standard method, not more than 0.001%.

Take an appropriate amount of 2-pyrrolidone, weigh it accurately, dissolve it with water and dilute it into a solution containing 5mg per lml as the test product solution. Take an appropriate amount of 2-pyrrolidone reference product, weigh it accurately, dissolve and dilute it with water to make a solution containing 0.1mg per 1ml as the reference solution. The method was determined by high performance liquid chromatography (general rule 0512) with octadecylsilane bonded silica gel as filler and water-acetonitrile-methanol as mobile phase (90:5:5) at the detection wavelength of 205nm. The reference solution of 20μl was precisely measured and injected into the liquid chromatograph, and the relative standard deviation of the peak area should not exceed 2.0%. Accurately measure 20μl each of the control solution and the test solution, inject them into the liquid chromatograph, record the chromatogram, and calculate the peak area according to the external standard method, not more than 2.0%.

Take 0.50g of formic acid, weigh it accurately, put it in 100ml bottle, dissolve it with mobile phase, dilute it to scale, shake well, and use it as test product solution. Take an appropriate amount of formic acid as the reference product, weigh it accurately, dissolve and dilute it with mobile phase to make a solution containing 25μg per 1ml as the reference product solution. The method was determined by high performance liquid chromatography (general rule 0512) with octadecylsilane bonded silica gel as filler and 0.01mol/L potassium dihydrogen phosphate solution acetonitrile (95:5) (pH adjusted to 3.0 by phosphoric acid) as mobile phase. The detection wavelength was 210nm. The separation degree of formic acid from adjacent peaks in the test solution should meet the requirements. Accurately measure 20μl each of the control solution and the test solution, inject them into the liquid chromatograph, record the chromatogram, and calculate the peak area according to the external standard method, not more than 0.5%.

Take 4.0g of this product (calculated as anhydrous matter), place it in a 100ml measuring bottle, dissolve it with water and dilute it to the scale, shake well, and use it as a reserve liquid. Precisely measure 25ml, add titanium trichloride – sulfuric acid solution 2.0ml, shake well, place for 30 minutes, as the test product solution. In addition, 25ml of the reserve liquid is precisely measured, 2.0ml of 13% sulfuric acid solution is added, shaken, and placed for 30 minutes, as a blank solution, according to UV-visible spectrophotometry (general rule 0401), the absorbance is measured at the wavelength of 405nm, not more than 0.35 (equivalent to 0.04% H2O2).

Take the hydrazine 2.5g of this product, weigh it accurately, put it in a 50ml centrifuge tube, add 25ml of water to dissolve, add 0.5ml of 5% salicylaldehyde methanol solution, shake well, heat it in a water bath at 60°C for 15 minutes, cool it, add toluene 2.0ml, tamper, shake vigorously for 2 minutes, centrifuge, and take the supernatant of the toluene layer as the test solution. In addition, an appropriate amount of salicylalazine was accurately weighed, dissolved with toluene and diluted to make a solution containing 9μg per 1ml as a control solution. According to thin layer chromatography (general rule 0502) test, absorb the above two solutions 10μl each, respectively, on the same dimethylsilanized silica thin layer plate, with methanol – water (2: 1) As a developing agent, unfold to the solvent front to 3/4 of the thin layer plate, take out, dry, and examine under ultraviolet lamp (365nm). The specific shift value (Rf) of salicylalazine is about 0.3. If the test solution shows fluorescence spots corresponding to the control solution, its fluorescence intensity should not be stronger than that of the control solution (0.0001%).

Moisture Take this product, according to the moisture determination method (general rule 0832) determination, moisture content shall not exceed 5.0%.

The residue shall be 1.0g of this product, inspected according to law (General rule 0841), and the residual residue shall not exceed 0.1%.

The residue left by heavy metals under the incandescing residue item shall be checked according to law (General Rule 0821 Second Law), and the heavy metals shall not exceed 10 parts per million.

Nitrogen content Take about 0.1g of this product, accurately weigh it, put it in Kjeldahl nitrogen determination bottle, add 10g potassium sulfate and 0.5g copper sulfate in turn, slowly add 20ml sulfuric acid along the wall of the bottle, put a small funnel in the Kjeldahl nitrogen determination bottle, slowly heat it with direct fire, the solution is clear green, continue heating for 30 minutes, cool. Transfer to 100ml bottle, dilute to scale with water and shake well. Precision absorption 10ml, according to the nitrogen determination method (general rule 0704 second method or third method) determination, the distillate with sulfuric acid titration solution (0.005mol/L) titration, and titration results with a blank test correction. According to anhydrous matter, the nitrogen content should be 11.5% ~ 12.8%.

[Category] Pharmaceutical excipients, adhesives and cosolvents, etc.

【 Storage 】 Dark, sealed storage.

Attached: Take 15% titanium trichloride solution (15g titanium trichloride dissolved in 100ml dilute hydrochloric acid) 20ml, carefully mix with 13ml sulfuric acid under ice bath, add appropriate amount of concentrated hydrogen peroxide solution until yellow, heat until white smoke, cool, dilute with water repeatedly and evaporate until the solution is nearly colorless, add water to obtain colorless solution. Add water to 100ml and shake well.

Note: This product is highly hygroscopic.