Meloxicam Tablets

General Notices

Action and use

Cyclo-oxygenase inhibitor; analgesic; anti-inflammatory.

Definition

Meloxicam Tablets contain Meloxicam.

The tablets comply with the requirements stated under Tablets and with the following requirements.

Content of meloxicam, C14H13N3O4S2

95.0 to 105.0% of the stated amount.

Identification

A. Carry out the method for thin-layer chromatography, Appendix III A, using the following solutions.
(1) To a quantity of the powdered tablets containing 50 mg of Meloxicam, add 5 mL of 0.1m methanolic sodium hydroxide and 20 mL of methanol, stir for 15 minutes and filter.
(2) Dissolve 50 mg of meloxicam BPCRS in 5 mL of 0.1m methanolic sodium hydroxide and add sufficient methanol to produce 25 mL of solution.
chromatographic conditions
(a) Use a silica gel F254 plate (Merck HPTLC plates are suitable).
(b) Use the mobile phase described below.
(c) Apply 10 µL of each solution.
(d) Develop the plate to 15 cm.
(e) After removal of the plate, dry in air and examine under ultraviolet light (254 nm).
mobile phase

1 volume of 13.5m ammonia, 20 volumes of methanol and 80 volumes of dichloromethane.

confirmation

The principal spot in the chromatogram obtained with solution (1) corresponds to that in the chromatogram obtained with solution (2).

B. In the Assay, the retention time of the principal peak in the chromatogram obtained with solution (1) is similar to that of the principal peak in the chromatogram obtained with solution (2).

Tests

Dissolution

Comply with the requirements for Monographs of the British Pharmacopoeia in the dissolution test for tablets and capsules, Appendix XII B1.

test conditions
(a) Use Apparatus 2, rotating the paddle at 50 revolutions per minute.
(b) Use 900 mL of a buffer prepared by dissolving 13.61 g of potassium dihydrogen orthophosphate in 800 mL of water, adjusting the pH to 7.5 with 0.5m sodium hydroxide, adding sufficient water to produce 1000 mL, at a temperature of 37°, as the medium.
procedure
(1) After 45 minutes, withdraw a sample of the medium and filter. Measure the absorbance of the filtrate, Appendix II B, diluted with the dissolution medium if necessary, at 362 nm using dissolution medium in the reference cell.
(2) Measure the absorbance of a solution prepared by dissolving 30 mg of meloxicam BPCRS in 5 mL of methanol, adding 1 mL of 0.1m sodium hydroxide and adding sufficient dissolution medium to produce 100 mL. Dilute a volume of the resulting solution with sufficient dissolution medium to produce a solution containing 0.00075% w/v of Meloxicam.
determination of content

Calculate the total content of Meloxicam, C14H13N3O4S2, in the medium from the absorbances obtained using the declared content of C14H13N3O4S2 in meloxicam BPCRS.

Related substances

Carry out the method for liquid chromatography, Appendix III D, using the following solutions.

(1) Moisten a quantity of powdered tablets containing 30 mg of Meloxicam with 10 mL of 1m sodium hydroxide, add 40 mL of methanol and mix with the aid of ultrasound for 5 minutes. Add 40 mL of methanol (40%), mix for 3 hours using a magnetic stirrer and then with the aid of ultrasound for 5 minutes. Cool, add sufficient methanol (40%) to produce 100 mL and filter.
(2) Dilute 1 volume of solution (1) to 100 volumes with methanol (40%). Dilute 1 volume of the resulting solution to 10 volumes with methanol (40%).
(3) Add 0.3 mL of 1m sodium hydroxide and 1 mL of dimethylformamide to 40 mg of meloxicam impurity standard BPCRS and dilute with methanol (40%) to produce 10 mL.
chromatographic conditions
(a) Use a stainless steel column (15 cm × 4.0 mm) packed with end-capped octadecylsilyl silica gel for chromatography (5 µm) (Inertsil ODS 2 is suitable).
(b) Use gradient elution and the mobile phase described below.
(c) Use a flow rate of 1.0 mL per minute.
(d) Use an ambient column temperature.
(e) Use detection wavelengths of 260 nm and 350 nm.
(f) Inject 10 µL of each solution.
mobile phase

Mobile phase A0.1% w/v of potassium dihydrogen orthophosphate adjusted to pH 6.0 with 2m sodium hydroxide.

Mobile phase Bmethanol.

system suitability

The test is not valid unless, in the chromatogram obtained with solution (3):

the chromatogram closely resembles the chromatogram supplied with meloxicam impurity standard BPCRS at 260 nm and 350 nm;

the resolution between the peaks due to meloxicam and impurity A at 350 nm is at least 3.0;

the resolution between the peaks due to impurity B and meloxicam at 260 nm is at least 3.0.

limits

In the chromatogram obtained with solution (1):

identify any peak corresponding to impurity A at 350 nm and multiply the area of this peak by a correction factor of 2.0;

the area of any peak corresponding to impurity A at 350 nm is not greater than twice the area of the principal peak in the chromatogram obtained with solution (2) (0.2%);

the area of any peak corresponding to impurity B at 260 nm is not greater than 1.5 times the area of the principal peak in the chromatogram obtained with solution (2) (0.15%).

In both the chromatograms obtained with solution (1) at 350 nm and at 260 nm:

the area of any other secondary peak is not greater than twice the area of the principal peak in the chromatogram obtained with solution (2) at that wavelength (0.2%).

The nominal total content of all such impurities is not greater than 0.5%.

Disregard any peak with an area less than the area of the principal peak in the chromatogram obtained with solution (2) at the same wavelength (0.1%).

Assay

Weigh and powder 20 tablets. Carry out the method for liquid chromatography, Appendix III D, using the following solutions.

(1) Moisten a quantity of the powdered tablets containing 30 mg of Meloxicam with 10 mL of 1m sodium hydroxide, add 40 mL of methanol and mix with the aid of ultrasound for 5 minutes. Add a further 40 mL of methanol, mix for 3 hours using a magnetic stirrer and then with the aid of ultrasound for 5 minutes. Cool, add sufficient methanol to produce 100 mL and filter.
(2) Dissolve 30 mg of meloxicam BPCRS in 10 mL of 1m sodium hydroxide and 40 mL of methanol, cool and add sufficient methanol to produce 100 mL.
(3) Add 0.3 mL of 0.4m sodium hydroxide to 40 mg of meloxicam impurity standard BPCRS and dilute with methanol (40%) to produce 10 mL.
chromatographic conditions

The chromatographic conditions described under Related substances may be used with a detection wavelength of 350 nm.

system suitability

The Assay is not valid unless, in the chromatogram obtained with solution (3):

the chromatogram closely resembles the chromatogram supplied with meloxicam impurity standard BPCRS;

the resolution between the peaks due to meloxicam and impurity A is at least 3.0.

determination of content

Calculate the content of C14H13N3O4S2 in the tablets using the declared content of C14H13N3O4S2 in meloxicam BPCRS.

Impurities

The impurities limited by the requirements of this monograph include those listed under Meloxicam.