Lansoprazole Delayed-Release Capsules
» Lansoprazole Delayed-Release Capsules contain not less than 90.0 percent and not more than 110.0 percent of the labeled amount of lansoprazole (C16H14F3N3O2S).
Packaging and storage— Preserve in tight containers, and store at controlled room temperature.
Identification—
A: Ultraviolet Absorption 197U
Medium: methanol.
Procedure— Powder a portion of Capsule contents equivalent to 5 mg of lansoprazole. Add 5 mL of methanol, shake well, and centrifuge. To 0.1 mL of the supernatant, add 10 mL of methanol.
B: The retention time of the major peak in the chromatogram of the Assay preparation corresponds to that in the chromatogram of the Standard preparation, as obtained in the Assay.
Dissolution 711 Proceed as directed for Procedure for Method A under Apparatus 1 and Apparatus 2, Delayed-Release Dosage Forms.
acid stage
Acid stage medium: 0.1 N hydrochloric acid; 500 mL.
Apparatus 2: 75 rpm.
Time: 60 minutes.
Procedure— Withdraw a 25-mL aliquot and then proceed immediately as directed for Test solution in the Buffer stage, leaving the remaining 475 mL in the vessel for use in the Buffer stage. Using a filtered portion of the aliquot, determine the amount of C16H14F3 N3O2S dissolved by employing UV absorption at the wavelength of maximum absorbance at about 306 nm, using Acid stage medium as the blank. Concomitantly determine the absorbance of the Acid stage test solution in comparison with a Standard solution of USP Lansoprazole RS having a known concentration equivalent to about 8% of the labeled amount of lansoprazole dissolved per 500 mL of Acid stage medium. [note—A volume of methanol not to exceed 0.5% of the total volume of the Standard solution may be used to dissolve USP Lansoprazole RS prior to dilution with Acid stage medium.]
Tolerances— Not more than 10% of the labeled amount of C16H14F3N3O2S is dissolved in 60 minutes.
buffer stage
Buffer concentrate— Transfer 65.4 g of monobasic sodium phosphate, 28.2 g of sodium hydroxide, and 12 g of sodium dodecyl sulfate to a suitable container, and add enough water to dissolve. Dilute with water to 4 L, and mix well.
Blank solution— Prepare a mixture of Acid stage medium and Buffer concentrate (19:17). Adjust, if necessary, with either phosphoric acid or sodium hydroxide to a pH of 6.8.
Test solution— Add 425 mL of Buffer concentrate to the remaining 475 mL of solution in each vessel from the Acid stage. Adjust, if necessary, with either phosphoric acid or sodium hydroxide to a pH of 6.8.
Apparatus 2: 75 rpm.
Time: 60 minutes.
Procedure— Determine the amount of C16H14F3N3O2S dissolved in filtered portions of the Test solution, using the difference between the absorbances at the wavelengths of about 286 nm and 650 nm, with Blank solution as the blank. Concomitantly determine the absorbances of the Test solution in comparison with a Standard solution of USP Lansoprazole RS having a known concentration equivalent to about 70% of the labeled amount of lansoprazole dissolved in 900 mL of Blank solution. [note—An amount of methanol not to exceed 2% of the total volume of the Standard solution may be used to dissolve USP Lansoprazole RS prior to dilution with Blank solution.]
Tolerances— Not less than 80% (Q) of the labeled amount of C16H14F3N3O2S is dissolved in 60 minutes.
Uniformity of dosage units 905: meet the requirements.
procedure for content uniformity
Test solution— Transfer the contents of 1 Capsule to a 100-mL volumetric flask, add 30 mL of 0.1 M sodium hydroxide, and sonicate to disintegrate. Add 65 mL of acetonitrile, cool, and dilute with acetonitrile to volume. Centrifuge a portion of the suspension and pass through a membrane filter having a 0.5-µm or finer porosity. Quantitatively dilute a volume of the filtrate with a mixture of acetonitrile and 0.1 M sodium hydroxide (7:3) to obtain a solution containing about 0.012 mg of lansoprazole per mL.
Procedure— Concomitantly determine the absorbances of the Test solution and a solution of USP Lansoprazole RS in the same medium and having a known concentration of about 0.012 mg of lansoprazole per mL, in 1-cm cells, at the wavelength of maximum absorbance at about 294 nm, with a suitable spectrophotometer, using a mixture of acetonitrile and 0.1 M sodium hydroxide (7:3) as the blank. Calculate the quantity, in mg, of C16H14F3N3O2S in the Capsule taken by the formula:
(LC/D)(AU / AS)
in which L is the labeled quantity of lansoprazole in the Capsule; C is the concentration, in mg per mL, of USP Lansoprazole RS in the Standard solution; D is the concentration, in mg per mL, of lansoprazole in the Test solution, based on the labeled quantity of lansoprazole per Capsule and the extent of dilution; and AU and AS are the absorbances of the Test solution and the Standard solution, respectively.
Loss on drying 731 Dry about 1 g of the Capsule contents in vacuum over phosphorus pentoxide at a pressure not exceeding 5 mm of mercury at 60 for 5 hours: it loses not more than 5.0% of its weight.
Assay—
Diluent, Mobile phase, and Resolution solution— Prepare as directed in the Assay under Lansoprazole.
Internal standard solution— Dissolve an accurately weighed quantity of 4¢-ethoxyacetophenone in acetonitrile to obtain a solution having a known concentration of about 7.5 mg per mL.
Standard preparation— Dissolve an accurately weighed quantity of USP Lansoprazole RS in a mixture of 0.1 M sodium hydroxide and acetonitrile (3:2) to obtain a solution having a known concentration of 3.0 mg per mL. Transfer 25.0 mL of this solution and 5.0 mL of Internal standard solution to a 50-mL volumetric flask, dilute with Diluent to volume, and mix. Quantitatively dilute with Diluent to obtain a solution having a known concentration of about 0.1 mg of USP Lansoprazole RS per mL.
Assay preparation— Transfer the contents of not fewer than 10 Capsules, equivalent to about 300 mg of lansoprazole, to a 300-mL conical flask containing 60.0 mL of 0.1 M sodium hydroxide, and sonicate until completely disintegrated. Add 20.0 mL of acetonitrile and 20.0 mL of Internal standard solution, shake well, and centrifuge a portion of the suspension. Quantitatively dilute a volume of the supernatant with Diluent to obtain a solution containing about 0.1 mg of lansoprazole per mL, and pass through a membrane filter having a 0.5-µm or finer porosity.
Chromatographic system (see Chromatography 621)— The liquid chromatograph is equipped with a 285-nm detector and a 4.6-mm × 25-cm column that contains 5-µm packing L1. The flow rate is about 1 mL per minute. Chromatograph the Resolution solution, and record the peak responses as directed for Procedure: the resolution, R, between the two major peaks is not less than 5. Chromatograph the Standard preparation, and record the peak responses as directed for Procedure: the relative standard deviation for replicate injections is not more than 2.0%.
Procedure— Separately inject equal volumes (about 10 µL) of the Standard preparation and the Assay preparation into the chromatograph, record the chromatograms, and measure the peak responses. Calculate the quantity, in mg, of lansoprazole (C16H14F3N3O2S) in each Capsule taken by the formula:
(LC/D)(RU / RS)
in which L is the labeled quantity, in mg, of lansoprazole in each Capsule taken; C is the concentration, in mg per mL, of USP Lansoprazole RS in the Standard preparation; D is the concentration, in mg per mL, of lansoprazole in the Assay preparation, based on the labeled quantity of lansoprazole in the Capsules taken and the extent of dilution; and RU and RS are the peak response ratios obtained from the Assay preparation and the Standard preparation, respectively.
Auxiliary Information— Please check for your question in the FAQs before contacting USP.
Topic/Question Contact Expert Committee
Monograph Elena Gonikberg, Ph.D.
Senior Scientist
1-301-816-8251
(MDGRE05) Monograph Development-Gastrointestinal Renal and Endocrine
Reference Standards Lili Wang, Technical Services Scientist
1-301-816-8129
RSTech@usp.org
711 Margareth R.C. Marques, Ph.D.
Senior Scientist
1-301-816-8106
(BPC05) Biopharmaceutics05
USP32–NF27 Page 2753
Pharmacopeial Forum: Volume No. 31(1) Page 161
Chromatographic Column—
Chromatographic columns text is not derived from, and not part of, USP 32 or NF 27.