Errata - English

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.

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%).

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 Analysis: Change
r_U = peak response of abiratrone acetate from the Sample solution
r_S = peak response of abiratrone acetate from the Standard solution
to:
r_U = peak response of abiraterone acetate from the Sample solution
r_S = peak response of abiraterone acetate from the Standard solution

In Detection solution: Change
Dissolve 1.25 g of potassium permanganate and 10.0 g of sodium hydroxide in 500 mL of water (prepared fresh for each plate), and heat at 105° for 5 min.
to:
Dissolve 1.25 g of potassium permanganate and 10.0 g of sodium hydroxide in 500 mL of water (prepared fresh for each plate).

In USP Atorvastatin Related Compound B RS: Change
(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)-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)(25)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)(25)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;

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;

In Related Compounds/Standard solution: Change
0.75 mg/mL of in water
to:
0.75 mg/mL of USP Filgrastim RS in water
AND
In Impurities with Charges Different from Filgrastim/Reference solution A: Change
1 mg/mL of in water
to:
1 mg/mL of USP Filgrastim RS in water
AND
In Impurities with Charges Different from Filgrastim/Reference solution B: Change
Dilute Reference solution A with water to obtain a concentration of 20 µg/mL of .
to:
Dilute Reference solution A with water to obtain a concentration of 20 µg/mL of USP Filgrastim RS.
AND
In Impurities with Charges Different from Filgrastim/Reference solution C: Change
3 mg/mL of in water
to:
3 mg/mL of USP Filgrastim RS in water
AND
In Impurities with Molecular Weight Different from That of Filgrastim/Reference solution A: Change
Dilute 25 µg of with 25 µL of 4X SDS sample buffer and sufficient water to obtain 100 µL of a solution containing a 250-µg/mL preparation of in 1X SDS sample buffer.
to:
Dilute 25 µg of USP Filgrastim RS with 25 µL of 4X SDS sample buffer and sufficient water to obtain 100 µL of a solution containing a 250-µg/mL preparation of USP Filgrastim RS in 1X SDS sample buffer.
AND
In Impurities with Molecular Weight Different from That of Filgrastim/Reference solution B: Change
Prepare both a reduced and a nonreduced Reference solution B by diluting Reference solution A (1:100) with the appropriate 1X SDS sample buffer to obtain a 2.5-µg/mL preparation of .
to:
Prepare both a reduced and a nonreduced Reference solution B by diluting Reference solution A (1:100) with the appropriate 1X SDS sample buffer to obtain a 2.5-µg/mL preparation of USP Filgrastim RS.
AND
In Impurities with Molecular Weight Different from That of Filgrastim/Reference solution C: Change
Dilute 75 µg of with 25 µL of 4X SDS sample buffer and sufficient water to obtain 100 µL of a solution containing a 750-µg/mL preparation of in 1X SDS sample buffer.
to:
Dilute 75 µg of USP Filgrastim RS with 25 µL of 4X SDS sample buffer and sufficient water to obtain 100 µL of a solution containing a 750-µg/mL preparation of USP Filgrastim RS in 1X SDS sample buffer.
AND
In Limit of High Molecular Weight Proteins/Resolution solution: Change
Dissolve about 1 mg of in 0.33 mL of 0.25 M sucrose,
to:
Dissolve about 1 mg of USP Filgrastim RS in 0.33 mL of 0.25 M sucrose,
AND
In Limit of High Molecular Weight Proteins/Standard solution: Change
0.3 mg/mL of in water
to:
0.3 mg/mL of USP Filgrastim RS in water

In Standard solution: Change
Prepare a solution containing 80 µg of and 200 µL of Digestion solution
to:
Prepare a solution containing 80 µg of USP Filgrastim RS and 200 µL of Digestion solution
AND
In System suitability requirements: Change
Eight major peaks should be present in each chromatogram as illustrated in the reference chromatogram provided with .
to:
Eight major peaks should be present in each chromatogram as illustrated in the reference chromatogram provided with USP Filgrastim RS.

In USP Reference Standards <11>/USP Ropivacaine Related Compound A RS: Change
2,6-Dimethylaniline hydrochloride.
C₈H₁₂ClN 157.64 [CAS-21436-98-6].
to:
2,6-Dimethylaniline hydrochloride.
C₈H₁₁N · HCl 157.64
AND
In USP Ropivacaine Related Compound B RS: Change
(R)-Ropivacaine hydrochloride monohydrate; (R)-(+)-1-propylpiperidine-2-carboxylic acid (2,6-dimethylphenyl)-amide hydrochloride monohydrate.
C₁₇H₂₆N₂O 328.89
to:
(R)-Ropivacaine hydrochloride monohydrate; (R)-(+)-1-propylpiperidine-2-carboxylic acid (2,6-dimethylphenyl)-amide hydrochloride monohydrate; (R)-N-(2,6-Dimethylphenyl)-1-propylpiperidine-2-carboxamide hydrochloride monohydrate.
C₁₇H₂₆N₂O · HCl · H₂O 328.88

In Analysis: Change
M = actual molarity of the Back-titrant (mM/mL)
to:
M = actual molarity of the Back-titrant (mmol/mL)
AND
Change
F = equivalency factor, 136.06 mg/mM
to:
F = equivalency factor, 136.06 mg/mmol

In USP Metoprolol Related Compound C RS: Change
(±)4-[2-Hydroxy-3-(1-methylethyl)aminopropoxy]benzaldehyde.
C₁₃H₁₉NO₃ 237.29
to:
4-[2-Hydroxy-3-(isopropylamino)propoxy]benzaldehyde hydrochloride.
C₁₃H₁₉NO₃ · HCl 273.76
AND
In USP Metoprolol Related Compound D RS: Change
(±) N,N-Bis[2-hydroxy-3-[4-(2-methoxyethyl)phenoxy]propyl](1-methylethyl)amine.
C₂₇H₄₁NO₆ 475.62
to:
N,N-Bis{2-hydroxy-3-[4-(2-methoxyethyl)phenoxy]propyl}isopropylamine hydrochloride; also known as (±) N,N-Bis[2-hydroxy-3-[4-(2-methoxyethyl)phenoxy]propyl](1-methylethyl)amine hydrochloride.
C₂₇H₄₁NO₆ · HCl 512.08

In Standard solution: Change
0.5 ng/mL of in Medium B.
to:
0.5 ng/mL of USP Filgrastim RS in Medium B.
AND
In Positive control solution: Change
10 ng/mL of in Medium B
to:
10 ng/mL of USP Filgrastim RS in Medium B

In USP Ropivacaine Related Compound A RS: Change
2,6-Dimethylaniline hydrochloride.
C₈H₁₂ClN 157.64
[CAS-21436-98-6].
to:
2,6-Dimethylaniline hydrochloride.
C₈H₁₁N · HCl 157.64
AND
In USP Ropivacaine Related Compound B RS: Change
(R)-Ropivacaine hydrochloride monohydrate; (R)-(+)-1-propylpiperidine-2-carboxylic acid (2,6-dimethylphenyl)-amide hydrochloride monohydrate.
C₁₇H₂₆N₂O 328.89
to:
(R)-Ropivacaine hydrochloride monohydrate; (R)-(+)-1-propylpiperidine-2-carboxylic acid (2,6-dimethylphenyl)-amide hydrochloride monohydrate; (R)-N-(2,6-Dimethylphenyl)-1-propylpiperidine-2-carboxamide hydrochloride monohydrate.
C₁₇H₂₆N₂O · HCl · H₂O 328.88

Change
Mobile phase: Acetonitrile, water, and 1 M ammonium formate (450:440:110), adding 0.19 mL of triethylamine to the acetonitrile portion
to:
Solution A: Add 0.19 mL of triethylamine to each 450 mL of acetonitrile.
Mobile phase: Solution A, water, and 1 M ammonium formate (450:440:110)

In the variable definition for F in Vitamin E, Method 2/Analysis: Change
1/2 for products labeled to contain all-rac vitamin E sources)
to:
1/2 (for products labeled to contain all-rac vitamin E sources)
AND
In Biotin, Method 2/Basal medium stock solution: Change
Dissolve the anhydrous dextrose and anhydrous Sodium acetate
to:
Dissolve the anhydrous dextrose and anhydrous sodium acetate
AND
In Cyanocobalamin, Method 2/Basal medium stock solution: Change
thedextros,
to:
the dextrose,
AND
In the Calculate statement in Niacin or Niacinamide, Pyridoxine Hydrochloride, Riboflavin, and Thiamine, Method 1/Analysis: Delete
, calcium pantothenate (C₁₈H₃₂CaN₂O₁₀), and folic acid (C₁₉H₁₉N₇O₆),
AND
In the Calculate statement in Niacin or Niacinamide, Pyridoxine Hydrochloride, Riboflavin, and Thiamine, Method 3/Analysis: Delete
, calcium pantothenate (C₁₈H₃₂CaN₂O₁₀), and folic acid (C₁₉H₁₉N₇O₆),
AND
In the Calculate statement in Folic Acid, Method 3; Ascorbic Acid, Niacin or Niacinamide, Pyridoxine Hydrochloride, Calcium Pantothenate, Riboflavin, and Thiamine, Method 4/Analysis: Add
ascorbic acid (C₆H₈O₆)

Change
Diluent 1—Prepare a solution of 0.1 mL of phosphoric acid in 1000 mL of water.
Diluent 2—Prepare a mixture of Diluent 1 and acetonitrile (60:40).
to:
Diluent 1—Prepare a solution of 0.1 mL of phosphoric acid in 1000 mL of water.

In Standard solution 3: Change
USP Methyl Caproate RS, USP Methyl Caprylate RS, USP Methyl Caprate RS, USP Methyl Laurate RS, and USP Methyl Laurate RS.
to:
USP Methyl Caproate RS, USP Methyl Caprylate RS, USP Methyl Caprate RS, USP Methyl Laurate RS, and USP Methyl Myristate RS.