Accessed from 128.83.63.

20 by nEwp0rt1 on Sun Nov 27 22:28:49 EST 2011

USP 35
citric acid solution, dilute with water to make 1000 mL, and mix. Mobile phasePrepare a suitable mixture of Buffer and methanol (55:45), and degas. Standard preparationDissolve an accurately weighed quantity of USP Piroxicam RS in 0.01 N methanolic hydrochloric acid to obtain a solution having a known concentration of about 0.25 mg per mL. Transfer 10.0 mL of this solution to a 50-mL volumetric flask, add about 25 mL of 0.01 N methanolic hydrochloric acid and 10.0 mL of water, dilute with 0.01 N methanolic hydrochloric acid to volume, and mix. This solution contains about 0.05 mg per mL. Assay preparationTransfer about 50 mg of Piroxicam, accurately weighed, to a 100-mL volumetric flask, dilute with 0.01 N methanolic hydrochloric acid to volume, and mix. Transfer 10.0 mL of this solution to a second 100-mL volumetric flask, add about 50 mL of 0.01 N methanolic hydrochloric acid and 20.0 mL of water, dilute with 0.01 N methanolic hydrochloric acid to volume, and mix. Chromatographic system (see Chromatography 621)The liquid chromatograph is equipped with a 254-nm detector and a 3.9-mm 30-cm column that contains packing L1. The flow rate is about 1.2 mL per minute. Chromatograph the Standard preparation, and record the peak responses as directed for Procedure: the column efficiency is not less than 500 theoretical plates, the tailing factor is not more than 1.5, and the relative standard deviation for replicate injections is not more than 2.0%. ProcedureSeparately inject equal volumes (about 25 L) of the Standard preparation and the Assay preparation into the chromatograph, record the chromatograms, and measure the responses for the major peaks. Calculate the quantity, in mg, of C15H13N3O4S in the portion of Piroxicam taken by the formula: 1000C(rU / rS) in which C is the concentration, in mg per mL, of USP Piroxicam RS in the Standard preparation, and rU and rS are the peak responses obtained from the Assay preparation and the Standard preparation, respectively.

Official Monographs / Piroxicam 4341

prepare the Standard solution, dissolve a suitable, accurately weighed quantity of USP Piroxicam RS in methanol to obtain a stock solution having a known concentration of about 0.5 mg per mL prior to dilution with Dissolution Medium.] TolerancesNot less than 75% (Q) of the labeled amount of C15H13N3O4S is dissolved in 45 minutes. Uniformity of dosage units 905: meet the requirements. Water, Method I 921: not more than 8.0%. Assay Buffer, Mobile phase, Standard preparation, and Chromatographic systemPrepare as directed in the Assay under Piroxicam. Assay preparationTransfer, as completely as possible, the contents of not less than 20 Capsules to a suitable tared container, and determine the average weight per capsule. Mix the combined contents, and transfer an accurately weighed portion, equivalent to about 50 mg of piroxicam, to a 100-mL volumetric flask. Add about 70 mL of 0.01 N methanolic hydrochloric acid, and shake by mechanical means for 30 minutes. Dilute with 0.01 N methanolic hydrochloric acid to volume, and mix. Centrifuge a portion of this mixture to obtain a clear solution. Transfer 10.0 mL of the solution so obtained to a 100-mL volumetric flask, add about 50 mL of 0.01 N methanolic hydrochloric acid and 20.0 mL of water, dilute with 0.01 N methanolic hydrochloric acid to volume, and mix. ProcedureProceed as directed for Procedure in the Assay under Piroxicam. Calculate the quantity, in mg, of C15H13N3O4S in the portion of the contents of Capsules taken by the formula: 1000C(rU / rS) in which C is the concentration, in mg per mL, of USP Piroxicam RS in the Standard preparation, and rU and rS are the peak responses obtained from the Assay preparation and the Standard preparation, respectively.

Piroxicam Cream
.

Piroxicam Capsules
.

Piroxicam Capsules contain not less than 92.5 percent and not more than 107.5 percent of the labeled amount of C15H13N3O4S.
Packaging and storagePreserve in tight, light-resistant containers. USP Reference standards 11 USP Piroxicam RS IdentificationDissolve a portion of the contents of Capsules in a mixture of chloroform and methanol (1:1) to obtain a solution containing about 1 mg per mL. Shake by mechanical means for 10 minutes, and filter a portion: the filtrate so obtained responds to Identification test C under Piroxicam. Dissolution 711 Medium: simulated gastric fluid TS, prepared without pepsin; 900 mL. Apparatus 1: 50 rpm. Time: 45 minutes. ProcedureDetermine the amount of C15H13N3O4S dissolved from UV absorbances at the wavelength of maximum absorbance at about 333 nm of suitably filtered portions of the solution under test, suitably diluted with Dissolution Medium, if necessary, in comparison with a Standard solution having a known concentration of USP Piroxicam RS in the same medium. [NOTEUse a suitable filter that does not adsorb piroxicam. To

Piroxicam Cream contains not less than 90.0 percent and not more than 110.0 percent of the labeled amount of piroxicam (C15H13N3O4S). Prepare Piroxicam Cream as follows (see Pharmaceutical CompoundingNonsterile Preparations 795): White Petrolatum . . . . . . . . . . . . . . Stearyl Alcohol . . . . . . . . . . . . . . . . Propylparaben . . . . . . . . . . . . . . . . Methylparaben . . . . . . . . . . . . . . . Propylene Glycol . . . . . . . . . . . . . . Sodium Lauryl Sulfate . . . . . . . . . . Sodium Hydroxide 1 N . . . . . . . . . Piroxicam . . . . . . . . . . . . . . . . . . . . Purified Water, a sufficient quantity to make . . . . . . . . . . . . . . . . . . . . 25 15 0.06 0.15 12.0 1 2.5 3 g g g g g g mL g

100 g

In an appropriate container (final weight tared), mix the White Petrolatum and Stearyl Alcohol together, and heat to 80 5 to form a clear oil phase. In a separate container, mix the Propylparaben, Methylparaben, Propylene Glycol, Sodium Lauryl Sulfate, and about 30 mL of Purified Water together, and heat to 80 5 to form a clear aqueous phase. Add the aqueous phase to

Official from May 1, 2012 Copyright (c) 2011 The United States Pharmacopeial Convention. All rights reserved.

Accessed from 128.83.63.20 by nEwp0rt1 on Sun Nov 27 22:28:49 EST 2011

4342 Piroxicam / Official Monographs

USP 35

the oil phase with continuous stirring, and allow it to cool to 50 to form an emulsion. In a mortar, triturate the Piroxicam with the Sodium Hydroxide to form a suspension. Using additional water to rinse out the mortar, add the Piroxicam suspension to the previously prepared emulsion, transferring the suspension stepwise and quantitatively to the emulsion. Add sufficient Purified Water with stirring to bring to final weight. Package and label.
Packaging and storagePreserve in a tight, light-resistant plastic resealable container, and store at controlled room temperature. LabelingLabel it to state the beyond-use date. USP Reference standards 11 USP Piroxicam RS Beyond-use date: 90 days at room temperature after the day on which it was compounded. Assay Buffer solutionDissolve 5.4 g of citric acid and 10.8 g of dibasic sodium phosphate in 2 L of Purified Water, and pass through a 0.45-m filter. Mobile phasePrepare a filtered and degassed mixture of Buffer solution and methanol (1:1). Make adjustments if necessary (see System Suitability under Chromatography 621). Diluent: 0.01 N methanolic hydrochloric acid, made by diluting 0.9 mL of hydrochloric acid with methanol to a volume of 1 L. Standard preparationDissolve an accurately weighed quantity of USP Piroxicam RS in 2 mL of chloroform, and dilute with Diluent to obtain a solution having a known concentration of about 50 g per mL. Assay preparationAdd about 340 mg of Piroxicam Cream to 4 mL of chloroform and 150 mL of Diluent. Shake the mixture on a wrist action shaker for 15 minutes, and dilute with Diluent to 200 mL. Pass the solution through a 0.45-m filter, and discard the first 5 mL of the filtrate. BlankPrepare as directed for the Assay preparation, without adding Piroxicam. Use Purified Water to offset the difference in weight between the Blank and the Assay preparation. Pass the solution through a 0.45-m filter, and discard the first 5 mL of the filtrate. Chromatographic system (see Chromatography 621)The liquid chromatograph is equipped with a 254-nm detector, a 4.6-mm 30-cm analytical column that contains 10-m packing L1, and a 4.6-mm 2-cm guard column that contains packing L1. The flow rate is about 1.0 mL per minute. Chromatograph the Standard preparation, and record the peak responses as directed for Procedure: the retention time is about 7 minutes, and the relative standard deviation for replicate injections is not more than 2.8%. ProcedureSeparately inject equal volumes (about 20 L) of the Standard preparation, the Assay preparation, and the Blank into the chromatograph, record the chromatograms, and measure the responses for the major peaks. Calculate the quantity, in mg, of piroxicam (C15H13N3O4S) in each mL of Piroxicam Cream taken by the formula: 200(C/V)(rU / rS) in which C is the concentration, in g per mL, of USP Piroxicam RS in the Standard preparation; V is the volume, in mL, of liquid taken; and rU and rS are the peak responses obtained from the Assay preparation and the Standard preparation, respectively.

Plantago Seed
.

DEFINITION Plantago Seed is the cleaned, dried, ripe seed of Plantago psyllium auct. or of Plantago indica L. (Plantago arenaria Waldst. & Kit.), known in commerce as Spanish or French psyllium; or of Plantago ovata Forssk., known in commerce as blond psyllium, or Indian plantago seed (Fam. Plantaginaceae). SPECIFIC TESTS BOTANIC CHARACTERISTICS Macroscopic Unground Plantago psyllium auct. seed: Ovate to ovateelongate, concavo-convex; mostly from 1.3 to 2.7 mm in length, rarely up to 3 mm, and from 600 m to 1.1 mm in width. It is light brown to moderate brown, darker along the margin, and very glossy; the convex dorsal surface exhibiting a lighter colored longitudinal area extending nearly the length of the seed and representing the embryo lying beneath the seed coat, and showing a sometimes indistinct transverse groove nearer the broader end. The concave ventral surface has a deep cavity, in the center of the base of which is an oval, yellowish white hilum. Unground Plantago indica seed: Ovate-oblong to elliptical, concavo-convex; from 1.6 to 3 mm in length and from 1 to 1.5 mm in width. Externally it is dark reddish brown to moderate yellowish brown, occasionally somewhat glossy, often dull, rough, and reticulate; the convex dorsal surface having a longitudinal lighter colored area extending lengthwise along the center and beneath the seed coat, and a median transverse groove, dent, or fissure. The ventral surface has a deep concavity, the edges somewhat flattened and frequently forming a sharp indented angle with the base of the cavity, the latter showing a light colored oval hilum. Unground Plantago ovata seed: Broadly elliptical to ovate, boat-shaped, from 2 to 3.5 mm in length and from 1 to 1.5 mm in width. It is pale brown to moderate brown with a dull surface, the convex surface having a small, elongated, glossy brown spot. The concave surface has a deep cavity, in the center of the base of which occurs a hilum covered with a thin membrane. Odor and taste: All varieties of Plantago Seed are nearly odorless. Microscopic: Plantago Seed is reniform in median transverse sections. Its seed coat has a colorless epidermis of mucilaginous cells whose radial and outer walls break down to form layers of mucilage when brought into contact with water, and a reddish brown to yellow pigment layer in the seeds of Plantago indica and Plantago psyllium, a broad endosperm with thick-walled outer palisade cells, and irregular inner endosperm cells; and a straight embryo extending lengthwise through the center. The endosperm and embryo cells contain fixed oil and aleurone grains, the latter being rounded, oval, pyriform, or irregularly shaped, from 2 to 8 m in diameter. WATER ABSORPTION Sample: 1 g of Plantago Seed Analysis: Place the Sample in a 25-mL graduated cylinder, add water to the 20-mL mark, and shake the cylinder at intervals during 24 h. Allow the seeds to settle for 12 h, and note the total volume occupied by the swollen seeds. Acceptance criteria: Seeds occupy the following volumes: Plantago psyllium, NLT 14 mL; Plantago ovata, NLT 10 mL; Plantago indica, NLT 8 mL. ARTICLES OF BOTANCAL ORIGIN, Foreign Organic Matter 561: NMT 0.50% ARTICLES OF BOTANICAL ORIGIN, Total Ash 561: NMT 4.0% ARTICLES OF BOTANCAL ORIGIN, Acid-Insoluble Ash 561: NMT 1.0% ADDITIONAL REQUIREMENTS PACKAGING AND STORAGE: Preserve in well-closed containers, secure against insect attack.

Official from May 1, 2012 Copyright (c) 2011 The United States Pharmacopeial Convention. All rights reserved.