Pharmaceutical grade cross-linked povidone experiment application research and development trial

Pharmaceutical grade cross-linked povidone experiment declared research and development of small test crovidone Jiaolian Juweitong Crospovidone This product is N-ethylene-2-pyrrolidone synthetic crosslinked water-insoluble homopolymer
.

The formula is (C6H9NO)n, where n represents the mean number of
1-vinyl-2-pyrrolidone links.

According to the calculation of anhydrous, the nitrogen content (N) should be 11.
0% to 12.
8%.
【Properties】This product is white or off-white powder
.

This product is insoluble in water, ethanol or in China
.

【Identification】(1) Take 1g of this product, add 10ml of water to shake to disperse into suspension, iodine test solution 0.
1ml, shake for 30 seconds, add starch indicator solution 1ml, shake, should be no blue generation
.

(2) The infrared light absorption pattern of this product should be consistent with the map of the control product (General Rule 0402
).

【Check】pH Take 1.
0g of this product, add 100ml of water and stir to make a uniform suspension, and determine according to law (General 0631), the pH value should be 5.
0 ~ 8.
0
.

Soluble matter in water Take 25.
0g of this product, put it in a beaker, add 200ml of water, stir for 1 hour, transfer it to a 250ml measuring flask with water, dilute it with water to the scale, shake well, let stand (generally not more than 24 hours), take the upper solution, centrifuge for 30 minutes (3500 rpm) per minute, take the supernatant filtered through the 0.
45 μm membrane, take 50ml of precision refill filtrate, place in a beaker that has been dried at 105 ° C for 3 hours and weighed, evaporated to dry, dried at 105 ° C for 3 hours, and the residual residue must not exceed 50mg (1.
0).
%）
。
N-ethylene-2-pyrrolidone Take about 1.
25g of this product, precision weighing, precision water 50ml, shaking to disperse, dense plug, shaking for 1 hour, after standing, take the supernatant filtered, continue the filtrate as a test solution; take N-ethylene-2-pyrrolidone control in an appropriate amount, precision weighing, dissolved with the mobile phase and diluted into a solution containing about 0.
25 μg per 1ml, as a control solution
.

Take N-ethylene-2-pyrrolidone control and vinyl acetate appropriate amount, dissolve with methanol and make a solution containing N-ethylene-2-pyrrolidone 1μg and vinyl acetate 50μg per 1ml as a system suitability solution
.

According to the high performance liquid chromatography (General Rule 0512), the detection wavelength is 235 nm
with octadecyl silane bonded silica gel as the filler and acetonitrile - water (8:92) as the mobile phase.

Take the system suitability solution 20μ1, inject into the liquid chromatography, record the chromatography, and the separation of the N-ethylene-2-pyrrolidone peak and the vinyl acetate peak should meet the regulations
.

Take 20 μl of the sample solution and the control solution with precision, inject it into the liquid chromatograph, record the chromatogram, and calculate the peak area according to the external standard method, which shall not exceed 0.
001%.
Peroxide Take 4.
0g of this product (calculated according to anhydrous), add 100ml of water and stir to make a uniform suspension as a storage solution
.

Precision amount of storage solution 25ml, add titanium trichloride - sulfuric acid solution 2.
0ml, shake well, leave for 30 minutes, as a test solution; another precision amount of storage solution 25ml, add sulfuric acid solution (13→100) 2.
0ml, shake well, place for 30 minutes, as a blank solution
.

According to ultraviolet-visible spectrophotometry (General 0401), the absorbance is determined at a wavelength of 405 nm, not more than 0.
35 (equivalent to 0.
04% H2O2).
Moisture Take this product, according to the moisture determination method (general rule 0832) to measure, the moisture content shall not exceed 5.
0%.
Blazing residue Take 2.
0g of this product, check according to law (General Rule 0841), and the residual residue shall not exceed 0.
1%.
Heavy metals Take the residue left under the incendiary residue and inspect it according to law (General Provisions 0821 Second Law), and the heavy metals shall not exceed 10
parts per million.

Arsenic salt Take 1.
0g of this product, put it in a Kjeldahl flask, add 5ml of sulfuric acid, heat it over low heat until completely carbonized (if necessary, sulfuric acid can be added, the total amount does not exceed 10ml), slowly drop and thicken the hydrogen peroxide solution, wait for the reaction to stop, continue to heat, and add concentrated hydrogen peroxide solution to the solution colorless, let it cool, add water for 10ml, evaporate to remove hydrogen peroxide, add 5ml of hydrochloric acid and water to an appropriate amount, check according to law (general rule 0822), should comply with the provisions (not more than 0.
0002%) ）
。
【Content determination】Take about 0.
2g of this product, weigh it precisely, determine it according to the nitrogen determination method (general rule 0704 first method or third method), calculate, that is, obtained
.

【Category】Pharmaceutical excipients, disintegrants and fillers, etc
.

【Storage】Protect from light, seal and preserve
.

【Labeling】The range
of the particle size distribution of this product should be indicated.