Errata - English

Change
Absence of Specified Microorganisms <2022>, Test Procedures, Test for Absence of Salmonella Species and Absence of Specified Microorganisms <2022>, Test Procedures, Test for Absence of Salmonella Species:
to:
Absence of Specified Microorganisms <2022>, Test Procedures, Test for Absence of Salmonella Species and Test for Absence of Escherichia coli:

In paragraph 3: Change
Upon completion of each ignition, cover the crucible, and allow it to cool in a desiccator to room temperature before weighing.
to:
Upon completion of each ignition, cover the crucible, and allow it to cool in a desiccator to room temperature before weighing accurately.

In In-Process Controls/paragraph 2: Change
Refer to Risk Assessment for discussion on critical process parameters (CPP).
to:
Refer to Quality Systems for discussion on critical process parameters (CPP).
AND
In Final Product Release Specifications/Dose-Defining Assays/paragraph 3: Change
relay
to:
rely

In USP Galantamine Hydrobromide Related Compounds Mixture RS: Change
Anhydrogalantamine;
(4aS,8aS)-3-Methoxy-11-methyl-9,10,11,12-tetrahydro-4aH-benzo[2,3]benzofuro[4,3-cd]azepine.
C₁₇H₁₉NO₂
to:
Anhydrogalantamine;
(4aS,8aS)-3-Methoxy-11-methyl-9,10,11,12-tetrahydro-4aH-benzo[2,3]benzofuro[4,3-cd]azepine.
C₁₇H₁₉NO₂ 269.34

Change
Mobile phase, Internal standard solution, and Standard preparation—Prepare as directed in the Assay under Theophylline.
to:
Buffer solution—Transfer 2.72 g of sodium acetate trihydrate to a 2000-mL volumetric flask, add about 200 mL of water, and shake until dissolution is complete. Add 10.0 mL of glacial acetic acid, dilute with water to volume, and mix.
Mobile phase—Transfer 70.0 mL of acetonitrile to a 1000-mL volumetric flask, dilute with Buffer solution to volume, and mix. Degas, and filter before using. Make adjustments if necessary (see System Suitability under Chromatography <621>).
Internal standard solution—Transfer about 50 mg of theobromine, accurately weighed, to a 100-mL volumetric flask, dissolve in 10.0 mL of 6 N ammonium hydroxide, dilute with Mobile phase to volume, and mix.
Standard preparation—Dissolve an accurately weighed quantity of USP Theophylline RS in Mobile phase, and dilute quantitatively, and stepwise if necessary, with Mobile phase to obtain a solution having a known concentration of about 1 mg per mL. Transfer 10.0 mL of this solution to a 100-mL volumetric flask, add 20.0 mL of Internal standard solution, dilute with Mobile phase to volume, and mix to obtain a solution having a known concentration of about 0.1 mg of USP Theophylline RS per mL.
AND
Change
Chromatographic system—Proceed as directed in the Assay under Theophylline.
to:
(see Chromatography <621>)—The liquid chromatograph is equipped with a 280-nm detector and a 4-mm × 30-cm 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 resolution, R, between the theophylline and theobromine peaks is not less than 2.0, the tailing factor for the theophylline peak is not more than 2.0, and the relative standard deviation for replicate injections is not more than 1.5%.
AND
Change
Procedure—Proceed as directed for Procedure in the Assay under Theophylline.
to:
Procedure—Separately inject equal volumes (between 10 µL and 25 µL) of the Standard preparation and the Assay preparation into the chromatograph, and measure the peak responses for the major peaks. The retention time of theophylline relative to that of theobromine is about 1.6.

Change
Homogenize 1 Capsule in 3 mL of water, add 3 mL of methanol, and centrifuge: the supernatant so obtained meets the requirements of the test for Radiochemical purity under Sodium Iodide I 123 Solution.
to:
Place a measured volume of a solution, containing 100 mg of potassium iodide, 200 mg of potassium iodate, and 1 g of sodium bicarbonate in each 100 mL, 25 mm from one end of a 25- × 300-mm strip of chromatographic paper (see Chromatography <621>), and allow to dry. To the same area add a similar volume of the sample solution prepared as follows: homogenize the content from 1 Capsule in 3 mL of water and 3 mL of methanol and centrifuge. The supernatant should be diluted so that it provides a count rate of about 20,000 counts per minute. Allow the spots to dry. Develop the chromatogram over a period of about 4 hours by ascending chromatography, using dilute methanol (7 in 10). Dry the chromatogram in air, and determine the radioactivity distribution by scanning with a suitable collimated radiation detector: the radioactivity of the iodide ¹²³I band is not less than 95.0% of the total radioactivity, and its R_F value falls within ±5.0% of the value found for sodium iodide when determined under similar conditions. Confirmation of the identity of the iodide band is made by the addition to the suspected iodide band of 6 drops of acidified hydrogen peroxide solution (prepared by adding 6 drops of 1 N hydrochloric acid to 10 mL of hydrogen peroxide solution) followed by the dropwise addition of starch TS: the development of a blue color indicates the presence of iodide.

Change
A solution or suspension of 1 or more Capsules in water responds to the test for Radionuclide identification under Sodium Iodide I 123 Solution.
to:
(see Radioactivity <821>)
The gamma-ray spectrum of a solution or suspension of 1 or more Capsules in water is identical to that of a specimen of ¹²³I of known purity that exhibits a major photoelectric peak having an energy of 0.159 MeV.

Change
pH 6.0 buffer, Mobile phase, Diluent, Standard preparation, Resolution solution, and Chromatographic system—Proceed as directed in the Assay under Carteolol Hydrochloride.
to:
Buffer, Mobile phase, Standard stock solution, Standard solution, System suitability stock solution, System suitability solution, Chromatographic system, and System suitability—
Proceed as directed in the Assay under Carteolol Hydrochloride.
AND
Add
Diluent—Prepare a mixture of Buffer and methanol (1:1).
AND
In all instances in Procedure: Change
Standard preparation
to:
Standard 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>.

Change
A solution or suspension of 1 or more Capsules in water responds to the test for Radionuclidic purity under Sodium Iodide I 123 Solution.
to:
(see Radioactivity <821>)
Using a suitable counting assembly, determine the radionuclidic purity of a solution or suspension of 1 or more Capsules in water: not less than 90% of the total radioactivity is present as I 123.

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.]

In Labeling: Change
as metoprolol succinate [(C₁₅H₂₅NO₃)₂ · C₄H₆O₆].
to:
as metoprolol tartrate [(C₁₅H₂₅NO₃)₂ · C₄H₆O₆].

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.]

In C: Change
It responds to Identification test C under Methyldopa.
to:
Sample: 10 mg
Analysis: To the Sample add 0.15 mL of a solution of ninhydrin in sulfuric acid (1 in 250): a dark purple color is produced within 5–10 min. Add 0.15 mL of water.
Acceptance criteria: The color changes to pale brownish yellow.

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
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
Anti-Factor Xa Activity for Low Molecular Weight Heparin
to:
The following procedure is used where specified in the individual monographs. This assay can be performed manually in plastic tubes utilizing heated block stations or water bath. Microtiter plate equipment with a reader and automated coagulometer can improve reproducibility and throughput. Acetic acid solution (stopping solution) is used for manual and microtiter plate assay. Automated coagulometers measure initial kinetic rate, and because of that, stopping of the reaction is not needed.
Anti-Factor Xa Activity for Low Molecular Weight Heparin

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.]

In Acceptance criteria: Change
The fluorescence intensity of the solution from the Sample solution is NMT 1.0% of the difference between the intensities of the two solutions.
to:
The fluorescence intensity of the solution from the Sample solution is NMT the difference between the intensities of the two solutions (NMT 1.0%).

In USP Atorvastatin Related Compound B RS: Change
3S,5R Isomer, or (3S,5R)-7-[3-(phenylcarbamoyl)-5-(4-fluorophenyl)-2-isopropyl-4-phenyl-1H-pyrrol-1-yl]-3,5-dihydroxyheptanoic acid, calcium salt.
to:
Calcium (3S,5R)-7-[2-(4-fluorophenyl)-5-isopropyl-3-phenyl-4-(phenylcarbamoyl)-1H-pyrrol-1-yl]-3,5-dihydroxyheptanoate (1:2); also known as 3S,5R Isomer, or (3S,5R)-7-[3-(phenylcarbamoyl)-5-(4-fluorophenyl)-2-isopropyl-4-phenyl-1H-pyrrol-1-yl]-3,5-dihydroxyheptanoic acid, calcium salt.

In Procedure: Change
694.83/676.83)(250)C_A(r_U/r_S)
in which 694.83 and 676.83 are the molecular weights of atropine sulfate monohydrate and anhydrous atropine sulfate, respectively;
to:
(694.84/676.82)(250)C_A(r_U/r_S)
in which 694.84 and 676.82 are the molecular weights of atropine sulfate monohydrate and anhydrous atropine sulfate, respectively;