Тест для переводчиков.

Тематика: регистрация лекарственного средства (фармакопея, аналитика, валидация процесса)

Appearance: yellow or brownish-yellow crystalline powder.

Nitrofurazone produced with the current process in ‘Jinda Ltd.’ has been analyzed with UV, IR, HNMR, CNMR and MS to confirm if the chemical structure is expected. The batch number used for this test is 20060601S, which is the working standard (WS) prepared from the current process, the USP RS (Lot: I0E149) was used as the reference material.

3.2.S.3.1.2.6 Chiral/Isomer

No asymmetric carbon atoms in the structure.

Test Method:

Test solution. Dissolve 0.10 g of the substance to be examined in the mobile phase and dilute to 100.0 ml with the mobile phase.

Reference solution (a). Dissolve 50.0 mg of (5-nitro-2-furyl)methylene diacetate R (impurity B) in the mobile phase and dilute to 100.0 ml with the mobile phase. Dilute 1.0 ml of this solution to 100.0 ml with the mobile phase.

Column: 250×4.6 mm, octadecylsilyl silica gel for chromatography R (5 μm);

Mobile phase: Acetonitrile-Water (4:6), adjust the pH of 3.0 with phosphoric acid;

Detection: 310 nm;

Flow rate: 1.0 ml/min;

Injection: 10 μl;

LOQ: 0.035% for (5-nitrofuran-2-yl)methylene diacetate, 126 ppm for Acetic acid

8. Accuracy

(1) Procedure

a) Choose LOD, 50%, 100%, 120% of the standard solution (four points).

Nitrofurazone（RRT=2.7min）+ 5-nitrofurfural (RRT=4.8min)+(5-nitrofuran-2-yl)methylene diacetate (RRT=10.5min)

A HPLC method was developed by ‘Jinda’ to determine this solvent in the final API. This method uses the C18 column. The whole method validation was performed, which include the System suitability, Specificity, Precision, Accuracy, Linearity, LOD and LOQ. The summary of validation result is listed in the following table.

Weigh accurately 0.1g of acetic acid to 100 ml of volumetric acid, dilute to mark with mobile phase, transfer 1 ml of this solution into test solution, and then dilute the test solution to mark with mobile phase. Ultrasonic, filter and inject.

Blank solution was prepared and injected. The noise of base line was calculated.

3.5 Repeatability

Inject the standard solution six times to calculate the average AUC of Acetic acid. Inject sample solution six times and calculate the added quantity of Acetic acid, average and RSD%.

ASSAY

Carry out the assay protected from bright light. Dissolve 60.0 mg in 20 ml of dimethylformamide R and dilute to 500.0 ml with water R. Dilute 5.0 ml to 100.0 ml with water R. Prepare a reference solution in the same manner using 60.0 mg of nitrofurazone RS. Measure the absorbances (2.2.25) of the two solutions at the maximum at 375 nm. Calculate the content of C₆H₆N₄O₄ from the absorbances measured and the concentrations of the solutions.

Loss on drying

Not more than 0.5 per cent, determined on 1.000 g by drying to constant weight in an oven at 105 °C.

Sulphated ash

Not more than 0.1 per cent, determined on 1.0 g.