Errata - English

Line 1: Change
Buffer solution and Mobile phase—Prepare as directed in the Assay under Diluted Isosorbide Dinitrate.
to:
Buffer solution and Mobile phase—Prepare as directed in the Assay.
AND
Line 1 of Chromatographic system: Change
(see Chromatography <621>)—Proceed as directed in the Assay under Diluted Isosorbide Dinitrate.
to:
(see Chromatography <621>)—Proceed as directed in the Assay.

Lines 6 and 7 of Procedure: Change
r_U × C_S × 900 × 100/r_S × D × LC
to:
r_U × C_S × 1000 × 100/r_S × D × LC
AND
Line 11 of Procedure: Change
900 is the volume
to:
1000 is the volume

Line 1: Change
Tablets respond to the Identification test under Isosorbide Dinitrate Tablets.
to:
Transfer a suitable quantity of finely powdered Tablets to a glass-stoppered centrifuge tube. Add 10 mL of sodium hydroxide solution (1 in 250), shake to wet the powder, then add 15 mL of solvent hexane, and again shake. Centrifuge the mixture, and transfer the upper phase to a beaker. Evaporate the solvent, and dry the residue in vacuum over anhydrous calcium chloride at room temperature for 16 hours: the IR absorption spectrum of a suitable solution in chloroform of the residue so obtained exhibits maxima only at the same wavelengths as that of a similar preparation from the residue obtained from USP Diluted Isosorbide Dinitrate RS.

Change
Weigh and powder a quantity of the Tablets, equivalent to about 250 mg of sotalol hydrochloride, and transfer to a 50-mL volumetric flask. Add 25 mL of methanol, and shake for 10 minutes. Dilute with methanol to volume, mix, and filter: the filtrate so obtained meets the requirements for Identification test B under Sotalol Hydrochloride.
to:
Thin-Layer Chromatographic Identification Test <201>—
Test solution—Weigh and powder a quantity of the Tablets, equivalent to about 250 mg of sotalol hydrochloride, and transfer to a 50-mL volumetric flask. Add 25 mL of methanol, and shake for 10 minutes. Dilute with methanol to volume, mix, and filter. Use the filtrate.
Developing solvent system: a mixture of chloroform and methanol (70:30).
Procedure—Proceed as directed in the chapter, except to place two 25-mL beakers, each containing about 10 mL of ammonium hydroxide, on the bottom of the chromatographic chamber that is lined with filter paper and contains the Developing solvent system, allow to equilibrate for 15 minutes, then place the plate in the chamber, and develop the chromatograms until the solvent front has moved about two-thirds of the length of the plate: meets the requirements.

Change
Mix a quantity of Oral Suspension, equivalent to about 200 mg of mebendazole, with 20 mL of a mixture of chloroform and 96 percent formic acid (19:1). Proceed as directed for Identification under Mebendazole Tablets, beginning with “Warm the suspension on a water bath for a few minutes.” The specified result is obtained.
to:
Mix a quantity of Oral Suspension, equivalent to about 200 mg of mebendazole, with 20 mL of a mixture of chloroform and 96 percent formic acid (19:1). Warm the suspension on a water bath for a few minutes, cool, and filter through a medium-porosity, sintered-glass filter. Apply 10 μL of this solution and 10 μL of a Standard solution of USP Mebendazole RS in a mixture of chloroform and 96 percent formic acid (19:1) containing 10 mg per mL to a suitable thin-layer chromatographic plate (see Chromatography <621>) coated with a 0.25-mm layer of chromatographic silica gel mixture. Allow the spots to dry, and develop the chromatogram in a solvent system consisting of a mixture of chloroform, methanol, and 96 percent formic acid (90:5:5) until the solvent front has moved about three-fourths of the length of the plate. Remove the plate from the developing chamber, mark the solvent front, allow the solvent to evaporate, and examine the plate under short-wavelength UV light: the R_F value of the principal spot obtained from the Test solution corresponds to that obtained from the Standard solution.

Change
Proceed as directed in the Identification test under Erythromycin Ethylsuccinate Oral Suspension, beginning with “Prepare a Standard solution.”
to:
Prepare a Standard solution of USP Erythromycin Ethylsuccinate RS in methanol containing about 3 mg per mL. Apply separately 10 µL each of the test solution and the Standard solution to a suitable thin-layer chromatographic plate (see Chromatography 〈621〉) coated with a 0.25-mm layer of chromatographic silica gel mixture, and allow to dry. Place the plate in an unlined chromatographic chamber, and develop the chromatograms in a solvent system consisting of a mixture of methanol and chloroform (85:15) until the solvent front has moved about 9 cm. Remove the plate from the chamber, mark the solvent front, and allow the solvent to evaporate. Spray the plate with a mixture of dehydrated alcohol, p-methoxybenzaldehyde, and sulfuric acid (90:5:5). Heat the plate at 100° for 10 minutes, and examine the chromatograms, in which the erythromycin and succinic acid moieties appear as black-to-purple spots: the R_F values of the principal spots obtained from the test solution correspond to those obtained from the Standard solution.

Line 1 of C: Change
Undiluted Oral Rinse used as the test solution meets the requirements for Identification test B under Calcium Gluconate, except that a Standard solution containing about 0.6 mg of USP Potassium Gluconate RS per mL is used and 15 μL of the test solution and the Standard solution are applied to the thin-layer chromatographic plate.
to:
Use undiluted Oral Rinse as the test solution and prepare a Standard solution of USP Potassium Gluconate RS in water containing 0.6 mg/mL. Apply separate 15-μL portions of the test solution and the Standard solution to a suitable thin-layer chromatographic plate (see Chromatography <621>) coated with a 0.25-mm layer of chromatographic silica gel, and allow to dry. Develop the chromatogram in a solvent system consisting of a mixture of alcohol, water, ammonium hydroxide, and ethyl acetate (50:30:10:10) until the solvent front has moved about three-fourths of the length of the plate. Remove the plate from the chamber, and dry at 110° for 20 minutes. Allow to cool and spray with a spray reagent prepared as follows. Dissolve 2.5 g of ammonium molybdate in about 50 mL of 2 N sulfuric acid in a 100-mL volumetric flask, add 1.0 g of ceric sulfate, swirl to dissolve, dilute with 2 N sulfuric acid to volume, and mix. Heat the plate at 110° for about 10 minutes: the principal spot obtained from the test solution corresponds in color, size, and R_F value to that obtained from the Standard solution.

Line 1: Change
Chewable Tablets respond to the Identification test under Isosorbide Dinitrate Tablets.
to:
Transfer a suitable quantity of finely powdered Tablets to a glass-stoppered centrifuge tube. Add 10 mL of sodium hydroxide solution (1 in 250), shake to wet the powder, then add 15 mL of solvent hexane, and again shake. Centrifuge the mixture, and transfer the upper phase to a beaker. Evaporate the solvent, and dry the residue in vacuum over anhydrous calcium chloride at room temperature for 16 hours: the IR absorption spectrum of a suitable solution in chloroform of the residue so obtained exhibits maxima only at the same wavelengths as that of a similar preparation from the residue obtained from USP Diluted Isosorbide Dinitrate RS.

Line 1: Change
A volume of Ophthalmic Solution, equivalent to about 2.5 mg of oxymetazoline hydrochloride, responds to the Identification test under Oxymetazoline Hydrochloride Nasal Solution.
to:
Place a volume of Ophthalmic Solution, equivalent to about 2.5 mg of oxymetazoline hydrochloride, in a 60-mL separator, and add water to make about 10 mL. Add 2 mL of sodium carbonate solution (1 in 10), extract with 10 mL of chloroform, and transfer the chloroform extract to a second 60-mL separator. Extract the chloroform solution with 10 mL of 0.1 N hydrochloric acid, allow to separate, and discard the chloroform layer. Transfer 8 mL of the acidic aqueous layer to a test tube, neutralize by the dropwise addition of 1 N sodium hydroxide, add 1 drop of 1 N sodium hydroxide in excess, and mix. Add a few drops of sodium nitroferricyanide TS and 2 drops of sodium hydroxide solution (15 in 100), mix, and allow to stand for 10 minutes. Add 0.1 N hydrochloric acid dropwise until the pH is between 8 and 9, and allow to stand for 10 minutes. A violet color develops.

In A.: Change
Render the filtrate alkaline with 6 N ammonium hydroxide, extract with several small portions of chloroform, and proceed as directed in Identification test A under Codeine Phosphate Injection, beginning with “Evaporate the combined chloroform extracts.” The specified results are observed.
to:
Render the filtrate alkaline with 6 N ammonium hydroxide and extract with several small portions of chloroform. Evaporate the combined chloroform extracts on a steam bath to dryness, and dry at 80° for 4 hours: the IR absorption spectrum of a potassium bromide dispersion of the residue so obtained exhibits maxima at the same wavelengths as that of the codeine obtained by similarly treating 1 mL of a solution of USP Codeine Phosphate RS (1 in 100).

Change
Proceed as directed in Identification test A under Metaproterenol Sulfate Inhalation Solution, beginning with “Allow the spots to dry”:
to:
Allow the spots to dry, and develop the chromatogram in a solvent system consisting of the upper layer of a freshly prepared mixture of butyl alcohol, water, and formic acid (50:25:7) until the solvent front has moved about three-fourths of the length of the plate. Remove the plate from the developing chamber, mark the solvent front, and allow the solvent to evaporate. Locate the spots on the plate by examination under short-wavelength UV light:

Change
Proceed as directed in Identification test A under Metaproterenol Sulfate Inhalation Solution, beginning with “Allow the spots to dry”:
to:
Allow the spots to dry, and develop the chromatogram in a solvent system consisting of the upper layer of a freshly prepared mixture of butyl alcohol, water, and formic acid (50:25:7) until the solvent front has moved about three-fourths of the length of the plate. Remove the plate from the developing chamber, mark the solvent front, and allow the solvent to evaporate. Locate the spots on the plate by examination under short-wavelength UV light:

In Cation-exchange column: Change
Proceed as directed under Column Partition Chromatography (see Chromatography 〈621〉),
to:
Proceed as directed under Chromatography 〈621〉, General Procedures, Column Chromatography,

Change
Mobile phase, Diluting solution, System suitability solution, and Chromatographic system—Prepare as directed in the test for Related compounds under Furosemide.
to:
Mobile phase—Prepare a filtered and degassed mixture of water, tetrahydrofuran, and glacial acetic acid (70:30:1). Make adjustments if necessary (see System Suitability under Chromatography <621>).
Diluting solution—Dilute 22 mL of glacial acetic acid with a mixture of acetonitrile and water (50:50) to 1000 mL, and mix.
System suitability solution—Dissolve suitable quantities of USP Furosemide RS and USP Furosemide Related Compound A RS in Diluting solution to obtain a solution containing about 20 µg per mL and 12 µg per mL, respectively.
Chromatographic system (see Chromatography <621>)—The liquid chromatograph is equipped with a detector capable of recording at both 254 nm and 272 nm and a 4.6-mm x 25-cm column that contains packing L1. [NOTE—The 2,4-dichloro-5-sulfamoylbenzoic acid impurity does not respond at 272 nm and the 2,4-bis(furfurylamino)-5-sulfamoylbenzoic acid impurity has a very intense absorbance at 254 nm.] The flow rate is about 1.0 mL per minute. Chromatograph the System suitability solution, and record the peak responses as directed for Procedure: the resolution, R, between furosemide and furosemide related compound A is not less than 2.5; and the relative standard deviation determined from furosemide is not more than 2.0%. [NOTE—The response for furosemide is at 254 nm.]

Change
Mobile phase, Diluting solution, System suitability solution and Chromatographic system—Prepare as directed in the test for Related compounds under Furosemide.
to:
Mobile phase—Prepare a filtered and degassed mixture of water, tetrahydrofuran, and glacial acetic acid (70:30:1). Make adjustments if necessary (see System Suitability under Chromatography <621>).
Diluting solution—Dilute 22 mL of glacial acetic acid with a mixture of acetonitrile and water (50:50) to 1000 mL, and mix.
System suitability solution—Dissolve suitable quantities of USP Furosemide RS and USP Furosemide Related Compound A RS in Diluting solution to obtain a solution containing about 20 µg per mL and 12 µg per mL, respectively.
Chromatographic system (see Chromatography <621>)—The liquid chromatograph is equipped with a detector capable of recording at both 254 nm and 272 nm and a 4.6-mm x 25-cm column that contains packing L1. [NOTE—The 2,4-dichloro-5-sulfamoylbenzoic acid impurity does not respond at 272 nm and the 2,4-bis(furfurylamino)-5-sulfamoylbenzoic acid impurity has a very intense absorbance at 254 nm.] The flow rate is about 1.0 mL per minute. Chromatograph the System suitability solution, and record the peak responses as directed for Procedure: the resolution, R, between furosemide and furosemide related compound A is not less than 2.5; and the relative standard deviation determined from furosemide is not more than 2.0%. [NOTE—The response for furosemide is at 254 nm.]

Line 1 of Test preparation: Change
Use the Assay preparation, prepared as directed in the Assay.
to:
Transfer about 69 mg of Aminosalicylate Sodium, accurately weighed, to a 100-mL low-actinic volumetric flask, add 50 mL of Mobile phase, and swirl to dissolve. Add 10.0 mL of Internal standard solution, dilute with Mobile phase to volume, and mix.

Line 1 of Test solution: Change
Use the Assay preparation, prepared as directed in the Assay.
to:
Weigh and finely powder not fewer than 20 Tablets. Transfer an accurately weighed portion of the powder, equivalent to about 690 mg of aminosalicylate sodium, to a 100-mL low-actinic volumetric flask. Add 50 mL of Mobile phase, and shake for about 5 minutes. Dilute with Mobile phase to volume, and mix. Filter, and transfer 10.0 mL of the clear filtrate to a low-actinic, 100-mL volumetric flask containing 10.0 mL of Internal standard solution, dilute with Mobile phase to volume, and mix.

Change the subsection:
Mobile phase and Internal standard solution—Prepare as directed in the Assay under Aminosalicylic Acid.
to:
Mobile phase—Prepare as directed in the Assay under Aminosalicylic Acid.
Internal standard solution—Prepare a solution of sulfanilamide in Mobile phase having a concentration of about 5 µg per mL.

Line 1 of Test solution: Change
Use the Assay preparation, prepared as directed in the Assay.
to:
Weigh and finely powder not fewer than 20 Tablets. Transfer an accurately weighed portion of the powder, equivalent to about 500 mg of aminosalicylic acid, to a 100-mL low-actinic volumetric flask. Add 50 mL of Mobile phase, and shake for about 5 minutes. Dilute with Mobile phase to volume, and mix. Filter, and transfer 10.0 mL of the clear filtrate to a 100-mL low-actinic volumetric flask containing 10.0 mL of Internal standard solution, dilute with Mobile phase to volume, and mix.

Change
A 1-mL portion of the filtrate from Identification test B meets the requirements of the test for Limit of morphine under Codeine Phosphate.
to:
Dissolve about 50 mg of potassium ferricyanide in 10 mL of water, and add 1 drop of ferric chloride TS and a 1-mL portion of the filtrate from Identification test B: no blue color is produced immediately.

In Acceptance criteria/Total impurities: Change
NMT 2.5%. Disregard any peak below 0.05% of the peak area of fluocinolone acetonide from the Standard solution.
to:
NMT 2.5%. Disregard any peak below 0.05% of the peak area of fluocinolone acetonide from the Sample solution.

Change
Other requirements
A solution or suspension prepared by homogenizing 1 or more Capsules in water to yield a concentration of not less than 1 MBq (25 µCi) per mL meets the requirements of the Assay for radioactivity under Sodium Iodide I 123 Solution.
to:
Assay for radioactivity
Prepare a solution or suspension by homogenizing 1 or more Capsules in water to yield a concentration of not less than 1 MBq (25 µCi) per mL. Determine the radioactivity of the resulting solution using a suitable counting assembly, by use of a calibrated system as directed under Radioactivity <821>.