Phytomenadione Tablets

General Notices

Action and use

Vitamin K analogue.

Definition

Phytomenadione Tablets contain Phytomenadione.

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

Content of phytomenadione, C31H46O2

90.0 to 110.0% of the stated amount.

Identification

Shake a quantity of the powdered tablets containing 50 mg of Phytomenadione with 50 mL of absolute ethanol for 1 hour, allow to stand and dilute 5 mL of the clear supernatant liquid to 50 mL with absolute ethanol. The light absorption of the resulting solution, Appendix II B, in the range 230 to 350 nm exhibits a maximum at 328 nm and a minimum at 292 nm. Dilute a suitable volume of the solution with sufficient absolute ethanol to produce a solution containing 0.001% w/v of Phytomenadione. The light absorption of this solution, in the range 230 to 350 nm, exhibits maxima at 245, 249, 263 and 271 nm and minima at 256 nm and 266 nm.

Tests

Disintegration

The requirement for Disintegration does not apply to Phytomenadione Tablets.

Menadione

Carry out the following procedure in subdued light. Carry out the method for thin-layer chromatography, Appendix III A, using the following solutions.

(1) Disperse a quantity of the powdered tablets containing 50 mg of Phytomenadione in 5 mL of absolute ethanol with the aid of ultrasound for 5 minutes, add 15 mL of 2,2,4-trimethylpentane, shake for 1 minute, centrifuge and use the supernatant liquid.
(2) 0.0025% w/v of menadione in 2,4,4-trimethylpentane.
chromatographic conditions
(a) Use as the coating silica gel F254 (Merck silica gel 60 F254 plates are suitable).
(b) Use the mobile phase as described below.
(c) Apply 50 µL of each solution.
(d) Develop the plate to 15 cm.
(e) After removal of the plate, allow it to dry in air and examine under ultraviolet light (254 nm).
mobile phase

1 volume of methanol, 20 volumes of ether and 80 volumes of cyclohexane.

limits

Any secondary spot corresponding to menadione in the chromatogram obtained with solution (1) is not more intense than the spot in the chromatogram obtained with solution (2) (1%).

Assay

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

(1) Add 5 mL of 0.5m ammonia to a quantity of the powdered tablets containing 10 mg of Phytomenadione and mix with the aid of ultrasound for 5 minutes. Add 90 mL of ethanol (96%) and mix with the aid of ultrasound for 10 minutes. Shake for 10 minutes, add sufficient ethanol (96%) to produce 100 mL, centrifuge and use the clear supernatant layer.
(2) 0.01% w/v of phytomenadione BPCRS in the mobile phase.
chromatographic conditions
(a) Use a stainless steel column (20 cm × 4 mm) packed with octadecylsilyl silica gel for chromatography (5 µm) (Spherisorb ODS 1 is suitable).
(b) Use isocratic elution and the mobile phase described below.
(c) Use a flow rate of 1.5 mL per minute.
(d) Use an ambient column temperature.
(e) Use a detection wavelength of 254 nm.
(f) Inject 20 µL of each solution.
mobile phase

5 volumes of water and 95 volumes of ethanol (96%).

determination of content

Calculate the content of C31H46O2 in the tablets using the declared content of C31H46O2 in phytomenadione BPCRS.

Labelling

The label states that the tablets should be chewed before swallowing or allowed to dissolve slowly in the mouth.

When vitamin K1 tablets are prescribed or demanded, Phytomenadione Tablets shall be dispensed or supplied.