Medical grade asphatan experiment declared research and development test

Medical grade aspatan experiment declared research and development of aspatan Asipatan Aspartame This product is N-L-α-aspartyl-L-phenylalanine-1-methyl ester
.

According to the calculation of dried products, C14H18N2O5 should be 98.
0% ~ 102.
0%.


【Properties】This product is a white crystalline powder
.

This product is minimally soluble in water and insoluble
in ethanol, n-hexane or dichloromethane.

Specific curl Take this product, precision weighing, add 15mol/L formic acid solution to dissolve and quantitatively dilute to make a solution containing about 40mg per 1ml, and immediately determine according to law (General 0621), the specific curl is +14.
5° to +16.
5
.


。
【Identification】(1) The infrared light absorption pattern of this product should be consistent
with the control spectrum (spectral set 768 figure).

(2) Take 0.
1g of this product, place it in a 100ml measuring flask, dissolve it with ethanol ultrasound and dilute it to the scale, and determine it according to ultraviolet-visible spectrophotometry (General Rule 0401), and have maximum absorption
at wavelengths of 247nm, 252nm, 258nm and 264nm.

【Check】Acidity Take 1.
0g of this product, add 125ml of water to dissolve, and determine according to law (General 0631), the pH value should be 4.
5 ~ 6.
0
.

The color of the solution Take 0.
8g of this product, add 100ml of cold water to boil, sonicate it, take 10ml, check according to law, and compare with the yellow-green No.
1 standard colorimetric liquid (general 0901 first method), not deeper
.

Absorbance Take this product, precision weighing, dissolve with 2mol / L hydrochloric acid solution and quantitatively dilute to make a solution containing 10mg per 1ml, according to ultraviolet-visible spectrophotometry (general rule 0401), the absorbance is determined at a wavelength of 430nm, and the absorbance should not be greater than 0.
022
.

The relevant substances take this product, add dilution [water-methanol (9:1)] ultrasonic dissolution and make a solution containing about 5mg per 1ml, as a test solution; Precise amount of the test solution 1ml placed in a 100ml measuring bottle, diluted with dilution solution to the scale, shaken well, as a control solution; Another 5-benzyl-3,6-dioxy-2-acetic acid control is taken in an appropriate amount, dissolved with dilution and made into a solution containing 50 μg per 1ml as a control solution
.

According to the high performance liquid chromatography (general rule 0512), the octadecyl silane bonded silica gel is used as a filler; Take 5.
6g of potassium dihydrogen phosphate, add 820ml of water to dissolve, adjust the pH to 4.
3 with phosphoric acid, add methanol to dilute to 1000ml, as a mobile phase; the detection wavelength is 210nm, the flow rate is 2ml per minute, and the column temperature is 40 °C
.

Take L-phenylalanine and 5-benzyl-3,6-dioxy-2-acetic acid control each appropriate amount, dissolve and dilute with the above dilution to make a solution containing about 0.
1mg each 1ml as a system suitability solution, take 20μl of the system suitability solution into the liquid chromatograph, record the chromatography, L-phenylalanine peak and 5-benzyl-3,6-dioxy-2-acetic acid peak resolution meets the requirements
.

Precise dosing of 20 μl of the control solution, the control solution and the test solution were injected into the liquid chromatograph to record the chromatography
.

According to the external standard method calculated by the main peak area of the control solution, the content of 5-benzyl-3,6-dioxy-2-acetic acid shall not exceed 1.
0%; In addition to 5-benzyl-3,6-dioxy-2-acetic acid and aspartan peak, the sum of all peak areas in the test solution shall not be greater than 1.
5 times (1.
5%)
of the main peak area of the control solution.

Conductivity Take 0.
8g of this product, weigh it precisely, place it in a 100ml measuring bottle, add new boiling and cold water, ultrasound dissolve and dilute to the scale, shake well
.

The conductivity C1 of the solution was determined separately, and the water conductivity C2
of the test product was prepared.

Calculate the conductivity according to the following formula: C1-0.
992C2
.

Must not exceed 30 μS/cm
.

Loss on drying Take this product, dry at 105 ° C for 4 hours, and the weight loss shall not exceed 4.
5% (General 0831).


Blazing residue Take 1.
0g of this product, inspect according to law (General Rule 0841), and the residual residue shall not exceed 0.
2%.


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 0.
67g of this product, add calcium hydroxide 1.
0g, mix, add water 2ml, stir evenly, dry at 40 ° C, slowly burn to carbonize, and then burn at 500 ~ 600 ° C to make complete ash, put cold, add hydrochloric acid 8ml and water 23ml, check according to law (general rule 0822 first law), should comply with the provisions (0.
0003%)
.

【Content determination】Take about 0.
25g of this product, weigh it precisely, add 3ml of formatic acid and 50ml of glacial acetic acid, dissolve, according to potentiometric titration (general rule 0701), titrate with perchloric acid titration solution (0.
1mol/L), and correct
the titration result with a blank test.

Each 1 ml perchloric acid titration solution (0.
1 mol/L) corresponds to 29.
43 mg of C14H18N2O5
.

【Category】Pharmaceutical excipients, sweeteners and flavoring agents
.

【Storage】Sealed and stored
in a dry place.