Teneligliptin Tablets
Teneligliptin Tablets contain not less than 90.0 per cent and not more than 110.0 per cent of the stated amount of teneligliptin, C22H30N6OS.
Usual strength. 20 mg.
Identification
In the Assay, the principal peak in the chromatogram obtained with test solution corresponds to the peak in the chromatogram obtained with the reference solution.
Tests
Dissolution (2.5.2).
Apparatus No. 1,
Medium. 900 ml of water,
Speed and time. 50 rpm and 30 minutes.
Withdraw a suitable volume of the medium and filter.
Determine by liquid chromatography (2.4.14).
Test solution. The filtrate obtained as given above. Dilute the filtrate if necessary, with the dissolution medium.
Reference solution. A 0.00327 per cent w/v solution of teneligliptin hydrobromide hydrate RS in the dissolution medium.
Use chromatographic system as described under Assay.
Inject the reference solution. The test is not valid unless the theoretical plates is not less than 1000, the tailing factor is not more than 2.0 and the relative standard deviation for replicate injections is not more than 2.0 per cent.
Inject the reference solution and the test solution.
Calculate the content of C22H30N6OS in the medium.
- Not less than 70 per cent of the stated amount ofC22H30N6OS.
Related substances. Determine by liquid chromatography (2.4.14).
Solution A. Dissolve 1 g of 1-octane sulphonic acid sodium salt anhydrous in 900 ml of water. Adjust the pH 3.1 with dilute orthophosphoric acid and dilute to 1000 ml withwater.
Solution B. A mixture of 50 volumes of solution A and 50 volumes of solvent mixture.
Solvent mixture. A mixture of 20 volumes of water and 80 volumes of acetonitrile.
Test solution. Weigh and transfer intact tablets containing about 100 mg of teneligliptin in 250-ml volumetric flask. Add about 200 ml of solution B and sonicate. Further sonicate for 15 minutes with intermittent swirling. Cool and dilute to volume with solution B, filter.
Chromatographic system
– a stainless steel column, 25 cm x 4.6 mm, packed with octadecylsilane bonded to porous silica (5 µm) (Such as Peerless Basic),
– mobile phase. A: a mixture of 82 volumes of solution A and 18 volumes of acetonitrile,
B: a mixture of 50 volumes of solution A and 50 volumes of acetonitrile,
– a gradient programme using the conditions given below,
– flow rate: 1 ml per minute,
– spectrophotometer set at 248 nm,
– injection volume: 10 µl.
Time Mobile phase A Mobile phase B
(in min.) (per cent v/v) (per cent v/v )
0 52 48
5 52 48
30 0 100
31 52 48
40 52 48
The relative retention time with reference to teneligliptin for teneligliptin impurity A [1-(3-methyl -1-phenyl-5-pyrazolyl) piperazine] is about 0.52.
Inject the test solution. The area of peak corresponding to teneligliptin impurity A, multiplied with the correction factor 0.59 is not more than 1.0 per cent. The area of any other secondary peak is not more than 0.5 per cent and the sum of the areas of all the secondary peaks is not more than 2.0 per cent, calculated by area normalisation.
Other tests. Comply with the tests stated under Tablets.
Assay. Determine by liquid chromatography (2.4.14).
Solvent mixture. A mixture of 60 volumes of water and 40 volumes of acetonitrile.
Test solution. Weigh and transfer intact tablets containing about 100 mg of Teneligliptin in 500-ml volumetric flask. Add about 10 ml of water and sonicate. Add about 350 ml of the solvent mixture and sonicate for 15 minutes with intermittent swirling. Cool and dilute to volume with the solvent mixture, filter. Dilute 5.0 ml of this solution to 25.0 ml with the solvent mixture.
Reference solution. A 0.0059 per cent w/v solution of teneligliptin hydrobromide hydrate RS in the solvent mixture.
Chromatographic system
– a stainless steel column 15 cm × 4.6 mm, packed with octadecylsilane bonded to porous silica (5 µm) (such as Eurosphere II 100-5),
– mobile phase: a mixture of 60 volumes of a buffer solution prepared by dissolving 1.36 g of potassium dihydrogen phosphate and 1g of 1-octane sulphonic acid sodium salt monohydrate into 1000 ml of water, adjusted to pH 2.7 with orthophosphoric acid and 40 volumes of acetonitrile,
– flow rate: 1 ml per minute,
– spectrophotometer set at 246 nm,
– injection volume: 20 µl.
Inject the reference solution. The test is not valid unless the theoretical plates is not less than 1000, the tailing factor is not more than 2.0 and the relative standard deviation for replicate injections is not more than 2.0 per cent.
Inject the reference solution and the test solution.
Calculate the content of C22H30N6OS in the tablets.
Labelling. The label states the strength in terms of the equivalent amount of teneligliptin.