Source

This product is 1- (3-azabicyclic [3.3.0] octyl) -3-p-toluenesulfonylurea, calculated as a dry product, and contains not less than 98.5% C15H21N3O3S.

character

This product is a white crystalline or crystalline powder, odorless.

This product is soluble in chloroform, slightly soluble in methanol, slightly soluble in ethanol, and insoluble in water.

melting point

The melting point of this product (general rule 0612) is 162~166 ℃.

distinguish

1. Take this product, dissolve it in ethanol and dilute it to make it contain approximately 10% per 1mL μ The solution of g was determined by UV visible spectrophotometry (General Rule 0401) and showed maximum absorption at a wavelength of 228nm.

2. The infrared absorption spectrum of this product should be consistent with the control spectrum (spectrogram 629).

inspect

Related substances

Determine according to the high performance liquid chromatography method (General Rule 0512), and use the newly prepared method.

Test solution: Take about 50mg of this product, accurately weigh it, place it in a 50mL volumetric flask, add about 20mL of acetonitrile to dissolve, dilute with water to the mark, and shake well.

Control solution: Accurately measure an appropriate amount of the test sample solution, dilute it with 40% acetonitrile solution to produce a solution containing approximately 2 µ g per 1mL, and shake well.

Reference solution: Take an appropriate amount of Impurity I reference solution, accurately weigh it, add an appropriate amount of acetonitrile to dissolve, dilute with 40% acetonitrile solution to make a solution containing approximately 1 µ g per 1mL, and shake well.

System suitability solution: Take appropriate amounts of Gliclazide and Impurity I reference materials, add appropriate amounts of acetonitrile to dissolve, dilute with 40% acetonitrile solution to prepare a mixed solution containing approximately 5 µ g and 15 µ g per 1mL, and shake well.

Chromatographic conditions: Using octylsilane bonded silica gel as the filler, acetonitrile water triethylamine trifluoroacetic acid (40:60:0.1:0.1) as the mobile phase, detection wavelength at 235nm, injection volume of 20 μ L.

System suitability requirements: In the chromatogram of the system suitability solution, the number of theoretical plates calculated based on the Gliclazide peak should not be less than 3000, and the separation degree between the Gliclazide peak and impurity I peak should be greater than 1.8.

Determination method: Accurately measure the test solution, control solution, and control solution, inject them into a liquid chromatograph, and record the chromatogram until twice the retention time of the main component peak.

Limit: If there are chromatographic peaks in the chromatogram of the test solution that have the same retention time as the main peak of the reference solution, they should be calculated based on the external standard method and should not exceed 0.1% of the peak area. The peak area of other individual impurities should not be greater than 0.5 times the main peak area of the reference solution (0.1%), and the sum of the peak areas of other impurities should not be greater than the main peak area of the reference solution (0.2%).

Loss on drying

Take this product and dry it to constant weight at 105 ℃. The weight loss should not exceed 1.0% (general rule 0831).

Scorching residue

Take 1.0g of this product and inspect it according to the law (General Rule 0841). The residual residue should not exceed 0.1%.

heavy metal

Take the residue left under the scorching residue item and inspect it in accordance with the law (General Rule 0821, Second Law), with a heavy metal content not exceeding 10 parts per million.

Content determination

Take approximately 0.2g of this product, accurately weigh it, dissolve it in 50mL of glacial acetic acid, and titrate it with perchloric acid titrant (0.1mol/L) according to the potentiometric titration method (General Rule 0701). Correct the titration results with a blank test. Every 1mL of perchloric acid titrant (0.1mol/L) is equivalent to 32.34mg of C15H21N3O3S.

category

Hypoglycemic drugs.

Storage

Shading and sealed storage.