standard testing procedure terbutaline sulphate

Storage Requirements:
Store protected from light and moisture.

Sampling:
Sample equal quantity from each container / bag. Collect a minimum of 5g from each container/bag sample into individual,

self –sealing clear polythene bag kept in another clear self sealing polythene bag bearing ‘Sample for Analysis,lable.

After completion of sampling return rest sample on same container. Collect control sample in Pet Bottle/Glass Bottle.
Quantity of Composite Sample:

10 g

Quantity of individual Identification
0.0100 g from each and every container /bag.

Quantity of Control Sample:

2 X 10 g

Description: A white or almost white, crystalline powder; odourless or almost odourless.

Solubility: Freely soluble in water; slightly soluble in ethanol (95 per cent); practically insoluble in chloroform and in ether.

Identification: Test A may be omitted B, C and D are carried out. Tests B and C may be omitted if tests A and D are carried out.
A. By IR
B. Absorbance at about 276nm and 280nm.
C.In the test for related substances, the principal peak in the chromatogram obtained with the test
Solution corresponds to the peak in the chromatogram obtained with reference solution (a).
D. Gives reaction A sulphates.

Appearance of solution: Absorbance of a 2-cm layer at 400nm, not more than 0.11.

Acidity: Not more than 1.2ml of 0.01M sodium hydroxide is required to change the colour of the solution to yellow.

tert-Butylamino-3, 5-dihydroxyacetophenone: Absorbance at about 330nm.

Related Substances: In the chromatogram obtained with the test solution, the area of the peak due to terbutaline impurity C is not more than twice area of the corresponding peak in the chromatogram obtained with reference solution (a)(0.2 per cent), the area of any other secondary peaks in the chromatogram obtained with reference solution (b)(0.2 per cent). The sum of all the secondary peaks
Other than terbutaline impurity C is not more than twice the area of the principal peak in the
Chromatogram obtained with reference solution (b)(0.4 per cent). Ignore any peak with an area less than
0.1 times the area of the principal peak in the chromatogram obtained with reference solution (b)
(0.02 per cent).

Heavy Metals: NMT 25ppm

Loss on Drying: NMT 0.5% w/w at 105º for 3 hours.

Assay: 98.0% to 101.0%w/w on the dried basis.

Description: A white or almost white, crystalline powder; odourless or almost odourless.

Solubility: Freely soluble in water; slightly soluble in ethanol (95 per cent); practically insoluble in chloroform and in ether.

Identification:

Test A may be omitted B, C and D are carried out. Tests B and C may be omitted if tests A and D are carried out.
A. By IR
B. When examined in the range 230nm to 360nm a 0.007 per cent w/v solution in 0.1M hydrochloric
acid shows absorption maxima at about 276nm and 280nm, 0.46 to 0.49.
C. In the test for Related substances, the principal peak in the chromatogram obtained with the test
Solution corresponds to the peak in the chromatogram obtained with reference solution (a).
D. A 2.0 per cent w/v solution in carbon dioxide-free water gives reaction A of sulphates.

Appearance of solution: A 2.0 per cent w/v solution in carbon dioxide –free water is clear; absorbance of a 2 –cm layer at 400nm, not more than 0.11.

Acidity: Dissolve 0.2g in 10ml of carbon dioxide-free water and titrate with 0.01 M sodium hydroxide, using
methyl red solution as indicator. Not more than 1.2ml of 0.01M sodium hydroxide is required to change the colour of the solution to yellow.

Tert-Butylamino-3, 5-dihydroxyacetophenone: Absorbance of a 2 per cent w/v solution in 0.01M hydrochloric acid at about 330nm, not more than 0.50.

Related Substances: Determine by liquid chromatography

Test solution: Dissolve 75mg of the substance under examination 50.0 ml of the mobile phase.

Reference solution (a): Dissolve 7.5mg of 1-(3, 5- dihydroxyphenyl)-2-[(1, 1-dimethyl) amino] ethanone RS (terbutaline impurity C RS) and 22.5 mg of terbutaline sulphate RS in 50.0 ml of the mobile phase. Dilute 1.0 ml of this solution to 100.0 ml with the mobile phase.

Reference solution (b): Dilute 1.0 ml of the test solution to 50.0 ml with the mobile phase. Dilute 2.0 ml of this solution to 20.0 ml with the mobile phase.

Chromatographic system

– a stainless steel column 15cm x 4.6 mm, packed with endcappped octadecylsilane bonded to porous silica (5µm).
– Mobile phase. Dissolve 4.23g of sodium hexasulphonate in 770 ml of 0.5 M ammonium format in about 980 ml of water, adjusted to pH 3.0 by anhydrous formic acid and dilute to 1000 ml with water and add 230 ml of methanol,
– flow rate .1 ml per minute
– spectrophotometer set at 276nm
– Injection volume. 20µl.

Inject reference solution (a). The test is not valid unless the resolution between the peaks due to
Terbutaline impurity C and terbutaline is not less than 2.0.

In the chromatogram obtained with the test solution, the area of the peak due to terbutaline impurity C is not more than twice area of the corresponding peak in the chromatogram obtained with reference solution (a) (0.2 per cent), the area of any other secondary peaks in the chromatogram obtained with reference solution (b)(0.2 per cent). The sum of all the secondary peaks other than terbutaline impurity C is not more than twice the area of the principal peak in the chromatogram obtained with reference solution (b)(0.4 per cent). Ignore any peak with an area less than 0.1 times the area of the principal peak in the chromatogram obtained with reference solution (b) (0.02 per cent).

Heavy Metals: Mix 1.6g with 0.6g of anhydrous sodium sulphate and ignite without melting the sodium sulphate. Cool, add 3 ml of 2 M hydrochloric acid boil and dilute to 50 ml with water. Cool and filter, 25ml of the filtrate complies with the limit test for heavy metals, Method A (25ppm).

Loss on Drying: Determined on 1.0 g by drying in an oven at 105° for 3 hours.