Errata - English

In Chromatographic system: Change
The liquid chromatograph is equipped with a 216-nm detector and a 4.6-mm × 20-cm column that contains packing L10.
to:
The liquid chromatograph is equipped with a 216-nm detector and a 4.6-mm × 25-cm column that contains packing L10.

Change
Constitute Erythromycin Ethylsuccinate for Oral Suspension as directed in the labeling, and proceed as directed in the Assay under Erythromycin Ethylsuccinate Oral Suspension.
to:
Constitute Erythromycin Ethylsuccinate for Oral Suspension as directed in the labeling, and proceed as directed for erythromycin under Antibiotics—Microbial Assays 〈81〉, using an accurately measured volume of the reconstituted suspension, freshly mixed and free from air bubbles, blended for 4 ± 1 minutes in a high-speed glass blender jar with sufficient methanol to give a stock solution containing the equivalent of about 1 mg of erythromycin per mL. Dilute this stock solution quantitatively with Buffer B.3 to obtain a Test Dilution having a concentration assumed to be equal to the median dose level of the Standard.

Change
Each mL of 0.1 N perchloric acid is equivalent to 7.953 mg of C₄H₁₀N₂ · 2HCl.
to:
Each mL of 0.1 N perchloric acid is equivalent to 9.207 mg of C₄H₁₀N₂ · H₃PO₄.

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 2: Change
Mobile phase, Standard preparation, System suitability solution, and Chromatographic system—Prepare as directed in the Assay under Diphenhydramine Hydrochloride.
to:
Mobile phase—Prepare a solution of acetonitrile, water, and triethylamine (50: 50: 0.5), adjust with glacial acetic acid to a pH of 6.5, filter, and degas. Make adjustments if necessary (see System Suitability under Chromatography <621> ).
Standard preparation—Dissolve an accurately weighed quantity of USP Diphenhydramine Hydrochloride RS in water to obtain a solution having a known concentration of about 0.5 mg per mL.
AND
After the Assay preparation subsection: Add
System suitability solution—Dissolve about 5 mg of benzophenone in 5 mL of acetonitrile, dilute with water to 100 mL, and mix. Transfer 1.0 mL of this solution and 5 mg of diphenhydramine hydrochloride to a 10-mL volumetric flask, dilute with water to volume, and mix.
Chromatographic system (see Chromatography <621>)—The liquid chromatograph is equipped with a 254-nm detector and a 4.6-mm × 25-cm column that contains packing L10. The flow rate is about 1 mL per minute. Chromatograph the System suitability solution, and record the peak responses as directed for Procedure; the resolution, R, between the benzophenone and diphenhydramine peaks is not less than 2.0. Chromatograph replicate injections of the Standard preparation, and record the peak responses as directed for Procedure; the relative standard deviation is not more than 2.0%, and the tailing factor for the diphenhydramine hydrochloride peak is not more than 2.0.
AND
Line 1 of Procedure: Change
Proceed as directed for Procedure in the Assay under Diphenhydramine Hydrochloride.
to:
Separately inject equal volumes, about 10 μL, of the Standard preparation and the Assay preparation into the chromatograph, record the chromatograms, and measure the responses for the major peaks.

Change
Ammonium bicarbonate solution, Diluent, Solution A, Solution B, Mobile phase, Internal standard solution, Standard preparation, and Chromatographic system—Proceed as directed in the Assay under Dimenhydrinate Tablets.
to:
Ammonium bicarbonate solution—Dissolve 4 g of ammonium bicarbonate in 250 mL of water.
Diluent—Dissolve 4 g of ammonium bicarbonate in 200 mL of water. Add 50 mL of methanol, and mix.
Solution A—Dissolve 0.8 g of ammonium bicarbonate in 800 mL of water. Add 200 mL of methanol, filter, and degas.
Solution B—Dissolve 0.8 g of ammonium bicarbonate in 150 mL of water. Add 850 mL of methanol, filter, and degas.
Mobile phase—Use variable mixtures of Solution A and Solution B as directed for Chromatographic system. Make adjustments if necessary (see System Suitability under Chromatography 〈621〉).
Internal standard solution—Prepare a solution in methanol containing 2.0 mg of 2-hydroxybenzyl alcohol per mL.
Standard preparation—Accurately weigh about 50 mg of USP Dimenhydrinate RS, add about 5 mL of Ammonium bicarbonate solution and 20.0 mL of Internal standard solution, and mix. To 1 mL of this solution add about 9 mL of Diluent, and mix.
AND
Add
Chromatographic system (see Chromatography 〈621〉)—The liquid chromatograph is equipped with a 229-nm detector and a 4.6-mm × 25-cm column that contains packing L7. The flow rate is about 1.5 mL per minute. The chromatograph is programmed as follows.

Time (minutes), 0, 0–7.0, 7.0–7.1, 7.1–15, 15–15.1, 15.1–22.0
Solution A (%), 100, 100, 100→0, 0, 0→100, 100
Solution B (%), 0, 0, 0→100, 100, 100→0, 0
Elution, equilibration, isocratic, linear gradient, isocratic, linear gradient, isocratic

Chromatograph the Standard preparation, and record the peak areas as directed for Procedure: the relative retention times are about 0.3 for 8-chlorotheophylline, 0.5 for the internal standard, and 1.0 for diphenhydramine; the resolution, R, between 8-chlorotheophylline and the internal standard is not less than 4.5; and the relative standard deviation for replicate injections is not more than 2.0%.
AND
Change
Procedure—Proceed as directed for Procedure in the Assay under Dimenhydrinate Tablets.
to:
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 areas for the major peaks.

Change
Buffer solution, Mobile phase, Internal standard solution, Standard preparation, and Chromatographic system—Prepare as directed in the Assay under Diluted Isosorbide Dinitrate.
to:
Buffer solution—Dissolve 15.4 g of ammonium acetate in water, add 11.5 mL of glacial acetic acid, dilute with water to 1000 mL, and mix to obtain a solution having a pH of about 4.7.
Mobile phase—Mix 350 mL of water, 100 mL of Buffer solution, and 550 mL of methanol. Cool to room temperature, dilute with water to 1000 mL, mix, degas, and filter. Make adjustments if necessary (see System Suitability under Chromatography <621>.)
Internal standard solution—Transfer a quantity of diluted nitroglycerin to a suitable volumetric flask, add about 60% of the flask volume of methanol, sonicate for 5 minutes, and shake for 30 minutes. Dilute with methanol to volume to obtain a solution having a concentration of about 3 mg of nitroglycerin per mL, and mix. Allow any undissolved material to settle, filter, and store the filtrate in an airtight container.
Standard preparation—Transfer about 125 mg of recently mixed USP Diluted Isosorbide Dinitrate RS, accurately weighed, to a 50-mL volumetric flask, add about 30 mL of Mobile phase, shake for 30 minutes, dilute with Mobile phase to volume, and mix. Pipet 10 mL of the resulting solution into a 25-mL volumetric flask, and add 4.0 mL of Internal standard solution and 4 mL of dilute Buffer solution (1 in 10). Cool to room temperature, dilute with Mobile phase to volume, and mix to obtain a solution having a known concentration of about 0.25 mg of isosorbide dinitrate per mL, based on the quantity of USP Diluted Isosorbide Dinitrate RS weighed and the labeled content of isosorbide dinitrate. Pass a portion of this solution through a 0.45-µm filter.
AND
Add
Chromatographic system (see Chromatography <621>)—The liquid chromatograph is equipped with a 220-nm detector and a 4-mm × 25-cm column that contains packing L1. The flow rate is about 1 mL per minute. Chromatograph the Standard preparation, and record the peak responses as directed for Procedure: the resolution, R, between isosorbide dinitrate and nitroglycerin is not less than 2.0; and the relative standard deviation for replicate injections determined from the peak response ratios is not more than 2%. [Note—The relative retention times are about 0.75 for isosorbide dinitrate and 1.0 for nitroglycerin. The relative retention times for isosorbide mononitrates, if present, are about 0.38.]
AND
Line 1 of Procedure: Change
Proceed as directed for Procedure in the Assay under Diluted Isosorbide Dinitrate.
to:
Separately inject equal volumes (about 20 µL) of the Standard preparation and the Assay preparation into the chromatograph, record the chromatograms, and measure the responses for the major peaks.

Line 2: Change
Mobile phase, Standard preparation, System suitability solution, and Chromatographic system—Prepare as directed in the Assay under Diphenhydramine Hydrochloride.
to:
Mobile phase—Prepare a solution of acetonitrile, water, and triethylamine (50: 50: 0.5), adjust with glacial acetic acid to a pH of 6.5, filter, and degas. Make adjustments if necessary (see System Suitability under Chromatography <621>).
Standard preparation—Dissolve an accurately weighed quantity of USP Diphenhydramine Hydrochloride RS in water to obtain a solution having a known concentration of about 0.5 mg per mL.
AND
After the Assay preparation subsection: Add
System suitability solution—Dissolve about 5 mg of benzophenone in 5 mL of acetonitrile, dilute with water to 100 mL, and mix. Transfer 1.0 mL of this solution and 5 mg of diphenhydramine hydrochloride to a 10-mL volumetric flask, dilute with water to volume, and mix.
Chromatographic system (see Chromatography <621>)—The liquid chromatograph is equipped with a 254-nm detector and a 4.6-mm × 25-cm column that contains packing L10. The flow rate is about 1 mL per minute. Chromatograph the System suitability solution, and record the peak responses as directed for Procedure; the resolution, R, between the benzophenone and diphenhydramine peaks is not less than 2.0. Chromatograph replicate injections of the Standard preparation, and record the peak responses as directed for Procedure; the relative standard deviation is not more than 2.0%, and the tailing factor for the diphenhydramine hydrochloride peak is not more than 2.0.
AND
Line 1 of Procedure: Change
Proceed as directed for Procedure in the Assay under Diphenhydramine Hydrochloride.
to:
Separately inject equal volumes, about 10 μL, of the Standard preparation and the Assay preparation into the chromatograph, record the chromatograms, and measure the responses for the major peaks.

Line 2: Change
Mobile phase and Chromatographic system—Proceed as directed in the Assay under Triazolam.
to:
Mobile phase—Prepare a filtered and degassed mixture of acetonitrile, chloroform, butyl alcohol, water, and glacial acetic acid (850:80:50:20:0.5). Make adjustments if necessary (see System Suitability under Chromatography <621>).
AND
After the Assay preparation subsection: Add a new subsection
Chromatographic system (see Chromatography <621>)—The liquid chromatograph is equipped with a 254-nm detector and a 4.6-mm × 30-cm column that contains packing L3. The flow rate is about 2.0 mL per minute. Chromatograph the Standard preparation, and record the peak responses as directed under Procedure: the relative retention times are 1 for triazolam and about 1.4 for the internal standard, the resolution, R, between the internal standard and triazolam is not less than 2.0, and the relative standard deviation for replicate injections is not more than 2.0%.
AND
Line 4 of Procedure: Change
Calculate the quantity, in mg, of C₁₇H₁₂Cl₂N₄ in the portion of Triazolam taken by the formula:
to:
Calculate the quantity, in mg, of C₁₇H₁₂Cl₂N₄ in the portion of Tablets taken by the formula:
AND
Line 9 of Procedure: Change
R_U and R_S are the ratios of the internal standard peak area to the triazolam peak area obtained from the Assay preparation and the Standard preparation, respectively.
to:
R_U and R_S are the ratios of the triazolam peak area to the internal standard peak area obtained from the Assay preparation and the Standard preparation, respectively.

Line 2: Change
Potassium stock solution and Standard preparations—
to:
Standard stock solution and Standard solutions—
AND
Line 1 of Procedure: Change
for Procedure in the Assay under Potassium Chloride Oral Solution.
to:
for Instrumental conditions and Analysis in the Assay under Potassium Chloride Oral Solution, except use Assay preparation instead of Sample solution.

Line 2: Change
Mobile phase, Standard preparation, System suitability solution, and Chromatographic system—Prepare as directed in the Assay under Diphenhydramine Hydrochloride.
to:
Mobile phase—Prepare a solution of acetonitrile, water, and triethylamine (50: 50: 0.5), adjust with glacial acetic acid to a pH of 6.5, filter, and degas. Make adjustments if necessary (see System Suitability under Chromatography <621>).
Standard preparation—Dissolve an accurately weighed quantity of USP Diphenhydramine Hydrochloride RS in water to obtain a solution having a known concentration of about 0.5 mg per mL.
AND
After the Assay preparation subsection: Add
System suitability solution—Dissolve about 5 mg of benzophenone in 5 mL of acetonitrile, dilute with water to 100 mL, and mix. Transfer 1.0 mL of this solution and 5 mg of diphenhydramine hydrochloride to a 10-mL volumetric flask, dilute with water to volume, and mix.
Chromatographic system (see Chromatography <621>)—The liquid chromatograph is equipped with a 254-nm detector and a 4.6-mm × 25-cm column that contains packing L10. The flow rate is about 1 mL per minute. Chromatograph the System suitability solution, and record the peak responses as directed for Procedure; the resolution, R, between the benzophenone and diphenhydramine peaks is not less than 2.0. Chromatograph replicate injections of the Standard preparation, and record the peak responses as directed for Procedure; the relative standard deviation is not more than 2.0%, and the tailing factor for the diphenhydramine hydrochloride peak is not more than 2.0.
AND
Line 1 of Procedure: Change
Proceed as directed for Procedure in the Assay under Diphenhydramine Hydrochloride.
to:
Separately inject equal volumes, about 10 μL, of the Standard preparation and the Assay preparation into the chromatograph, record the chromatograms, and measure the responses for the major peaks.

Line 1: Change
Phosphate buffer, Mobile phase, and System suitability solution—Proceed as directed in the Assay under Vinorelbine Tartrate.
to:
Phosphate buffer—Dissolve 6.9 g of monobasic sodium phosphate in 900 mL of water. Adjust with phosphoric acid to a pH of 4.2, dilute with water to 1000 mL, and mix.
Mobile phase—Dissolve 1.22 g of sodium 1-decanesulfonate in 620 mL of methanol. Add 380 mL of Phosphate buffer, mix, filter, and degas. Make adjustments if necessary (see System Suitability under Chromatography <621>).
System suitability solution—Dissolve accurately weighed quantities of USP Vinorelbine Tartrate RS and USP Vinorelbine Related Compound A RS in water, and dilute quantitatively, and stepwise if necessary, with water to obtain a solution having known concentrations of about 1.4 mg per mL and 0.01 mg per mL, respectively. Expose a portion of this solution in a suitable xenon lamp apparatus capable of supplying a dose of 1600 KJ/m² between 310 and 800 nm at a power of 500 W/m² for about 1 h, in order to generate an additional degradation product 3,6-epoxy vinorelbine having a relative retention time of about 0.8.

In Chromatographic system: Change
Chromatograph the Standard preparation, and record the peak responses as directed for Procedure: the standard deviation for replicate injections is not more than 2.0%.
to:
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%.

In Procedure: Change
(336.48/528.59)CD(r_U/r_S)
in which 336.48 and 528.59 are the molecular weights
to:
(336.48/528.60)CD(r_U/r_S)
in which 336.48 and 528.60 are the molecular weights

Line 1 of Mobile phase and Chromatographic system: Change
Prepare as directed in the Assay under Trihexyphenidyl Hydrochloride.
to:
Mobile phase—Prepare a mixture of acetonitrile, water, and triethylamine (920:80:0.2), adjust with phosphoric acid to a pH of 4.0, mix, filter, and degas. Make adjustments if necessary (see System Suitability under Chromatography <621>).
Chromatographic system (see Chromatography <621>)—The liquid chromatograph is equipped with a 210-nm detector and a 4.6-mm × 8-cm column that contains 3-µm packing L1. The flow rate is about 2 mL per minute. Chromatograph the Standard preparation, and record the peak responses as directed for Procedure: the column efficiency determined from the analyte peak is not less than 1300 theoretical plates, the tailing factor for the analyte peak is not more than 3.0, and the relative standard deviation for replicate injections is not more than 1.0%.
AND
Line 1 of Procedure: Change
Proceed as directed for Procedure in the Assay under Trihexyphenidyl Hydrochloride.
to:
Separately inject equal volumes (about 10 µL) of the Standard preparation and the Assay preparation into the chromatograph, record the chromatograms, and measure the responses for the major peaks.
AND
Line 6 of Procedure: Change
and the other terms are as defined therein.
to:
C is the concentration, in mg per mL, of USP Trihexyphenidyl Hydrochloride RS in the Standard preparation, r_U and r_S are the trihexyphenidyl peak responses obtained from the Assay preparation and the Standard preparation, respectively.

Line 2: Change
Mobile phase, Standard preparation, Resolution solution, and Chromatographic system—Proceed as directed in the Assay under Minocycline Hydrochloride.
to:
Mobile phase—Prepare a mixture of 0.2 M ammonium oxalate, 0.01 M edetate disodium, dimethylformamide, and tetrahydrofuran (600:180:120:80). Adjust with ammonium hydroxide to a pH of 7.2, and pass through a filter of 0.5-µm or finer pore size. Make adjustments if necessary (see System Suitability under Chromatography <621>).
Standard preparation—Dissolve an accurately weighed quantity of USP Minocycline Hydrochloride RS in water to obtain a solution having a known concentration of about 500 µg of minocycline (C₂₃H₂₇N₃O₇) per mL. Use this solution within 3 hours.
Resolution solution—Transfer 10 mg of USP Minocycline Hydrochloride RS to a 25-mL volumetric flask, add 20 mL of 0.2 M ammonium oxalate, and swirl to dissolve. Heat on a water bath at 60° for 180 minutes, and allow to cool. Dilute with water to volume, and mix.
Chromatographic system (see Chromatography <621>)—The liquid chromatograph is equipped with a 280-nm detector and a 4.6-mm × 25-cm column that contains 5-µm packing L1, and is maintained at a constant temperature of about 40°. The flow rate is about 1.5 mL per minute. Chromatograph the Standard preparation, and record the peak responses as directed for Procedure: the capacity factor, k´, is not less than 5.0 and not more than 11.5; the tailing factor for the analyte peak is not less than 0.9 and not more than 2.0; and the relative standard deviation for replicate injections is not more than 2.0%. Chromatograph the Resolution solution, and record the peak responses as directed for Procedure: the relative retention times are about 0.7 for epiminocycline and 1.0 for minocycline; and the resolution, R, between epiminocycline and minocycline is not less than 4.6.
AND
Line 1 of Procedure: Change
Proceed as directed for Procedure in the Assay under Minocycline Hydrochloride.
to:
Separately inject equal volumes (about 20 µL) of the Standard preparation and the Assay preparation into the chromatograph, record the chromatograms, and measure the responses for the major peaks.

Change
Solution A, Solution B, Mobile phase, Internal standard solution, and Chromatographic system—Prepare as directed in the Assay under Dimenhydrinate Tablets.
to:
Solution A—Dissolve 0.8 g of ammonium bicarbonate in 800 mL of water. Add 200 mL of methanol, filter, and degas.
Solution B—Dissolve 0.8 g of ammonium bicarbonate in 150 mL of water. Add 850 mL of methanol, filter, and degas.
Mobile phase—Use variable mixtures of Solution A and Solution B as directed for Chromatographic system. Make adjustments if necessary (see System Suitability under Chromatography 〈621〉).
Internal standard solution—Prepare a solution in methanol containing 2.0 mg of 2-hydroxybenzyl alcohol per mL.
AND
Add
Chromatographic system (see Chromatography 〈621〉)—
The liquid chromatograph is equipped with a 229-nm detector and a 4.6-mm × 25-cm column that contains packing L7. The flow rate is about 1.5 mL per minute. The chromatograph is programmed as follows.

Time (minutes), 0, 0–7.0, 7.0–7.1, 7.1–15, 15–15.1, 15.1–22.0
Solution A (%), 100, 100, 100→0, 0, 0→100, 100
Solution B (%), 0, 0, 0→100, 100, 100→0, 0
Elution, equilibration, isocratic, linear gradient, isocratic, linear gradient, isocratic

Chromatograph the Standard preparation, and record the peak areas as directed for Procedure: the relative retention times are about 0.3 for 8-chlorotheophylline, 0.5 for the internal standard, and 1.0 for diphenhydramine; the resolution, R, between 8-chlorotheophylline and the internal standard is not less than 4.5; and the relative standard deviation for replicate injections is not more than 2.0%.
AND
Change
Procedure—Proceed as directed for Procedure in the Assay under Dimenhydrinate Tablets. Calculate the quantity, in mg, of dimenhydrinate (C₁₇H₂₁NO · C₇H₇ClN₄O₂) in each mL of the Injection taken by the formula:
(200C/V)(R_U/R_S)
in which C is the concentration of USP Dimenhydrinate RS in the Standard preparation; V is the volume, in mL, of Injection taken; and the other terms are as defined therein.
to:
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 areas for the major peaks. Calculate the quantity, in mg, of dimenhydrinate (C₁₇H₂₁NO · C₇H₇ClN₄O₂) in each mL of the Injection taken by the formula:
(200C/V)(R_U/R_S)
in which C is the concentration of USP Dimenhydrinate RS in the Standard preparation; V is the volume, in mL, of Injection taken; and R_U and R_S are the peak area ratios of diphenhydramine to the internal standard obtained from the Assay preparation and the Standard preparation, respectively.

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.

Line 1 of Mobile phase and Chromatographic system: Change
Prepare as directed in the Assay under TrihexyphenidylHydrochloride.
to:
Mobile phase—Prepare a mixture of acetonitrile, water, and triethylamine (920:80:0.2), adjust with phosphoric acid to a pH of 4.0, mix, filter, and degas. Make adjustments if necessary (see System Suitability under Chromatography <621>).
Chromatographic system (see Chromatography <621>)—The liquid chromatograph is equipped with a 210-nm detector and a 4.6-mm × 8-cm column that contains 3-µm packing L1. The flow rate is about 2 mL per minute. Chromatograph the Standard preparation, and record the peak responses as directed for Procedure: the column efficiency determined from the analyte peak is not less than 1300 theoretical plates, the tailing factor for the analyte peak is not more than 3.0, and the relative standard deviation for replicate injections is not more than 1.0%.
AND
Line 1 of Procedure: Change
Proceed as directed for Procedure in the Assay under Trihexyphenidyl Hydrochloride.
to:
Separately inject equal volumes (about 10 µL) of the Standard preparation and the Assay preparation into the chromatograph, record the chromatograms, and measure the responses for the major peaks.
AND
Line 7 of Procedure: Change
and the other terms are as defined therein.
to:
C is the concentration, in mg per mL, of USP Trihexyphenidyl Hydrochloride RS in the Standard preparation, r_U and r_S are the trihexyphenidyl peak responses obtained from the Assay preparation and the Standard preparation, respectively.

Change
Buffer solution, Mobile phase, Internal standard solution, Standard preparation, and Chromatographic system—Prepare as directed in the Assay under Diluted Isosorbide Dinitrate.
to:
Buffer solution—Dissolve 15.4 g of ammonium acetate in water, add 11.5 mL of glacial acetic acid, dilute with water to 1000 mL, and mix to obtain a solution having a pH of about 4.7.
Mobile phase—Mix 350 mL of water, 100 mL of Buffer solution, and 550 mL of methanol. Cool to room temperature,dilute with water to 1000 mL, mix, degas,and filter. Make adjustments if necessary (see System Suitability underChromatography <621>).
Internal standard solution—Transfer a quantity of diluted nitroglycerin to a suitable volumetric flask, add about 60% of the flask volume of methanol, sonicate for 5 minutes, and shake for 30 minutes. Dilute with methanol to volume to obtain a solution having a concentration of about 3 mg of nitroglycerin per mL, and mix. Allow any undissolved material to settle, filter, and store the filtrate in an airtight container.
Standard preparation—Transfer about 125 mg of recently mixed USP Diluted Isosorbide Dinitrate RS, accurately weighed, to a 50-mL volumetric flask, add about 30 mL of Mobile phase, shake for 30 minutes, dilute with Mobile phase to volume, and mix. Pipet 10 mL of the resulting solution into a 25-mL volumetric flask, and add 4.0 mL of Internal standard solution and 4 mL of dilute Buffer solution (1 in 10). Cool to room temperature, dilute with Mobile phase to volume, and mix to obtain a solution having a known concentration of about 0.25 mg of isosorbide dinitrate per mL, based on the quantity of USP Diluted Isosorbide Dinitrate RS weighed and the labeled content of isosorbide dinitrate. Pass a portion of this solution through a 0.45-µm filter.
AND
Change
Procedure—Proceed as directed for Procedure in the Assay under Diluted Isosorbide Dinitrate.
to:
Chromatographic system (see Chromatography <621>)—The liquid chromatograph is equipped with a 220-nm detector and a 4-mm × 25-cm column that contains packing L1. The flow rate is about 1 mL per minute. Chromatograph the Standard preparation, and record the peak responses as directed for Procedure: the resolution, R, between isosorbide dinitrate and nitroglycerin is not less than 2.0; and the relative standard deviation for replicate injections determined from the peak response ratios is not more than 2%. [NOTE—The relative retention times are about 0.75 for isosorbide dinitrate and 1.0 for nitroglycerin. The relative retention times for isosorbide mononitrates, if present, are about 0.38.]
Procedure—Separately inject equal volumes (about 20 µL) of the Standard preparation and the Assay preparation into the chromatograph, record the chromatograms, and measure the responses for the major peaks.

Line 1: Change
It meets the requirements of the test for Chromatographic purity under Albuterol, except to read Albuterol Sulfate in place of Albuterol and to use water instead of methanol as the solvent to prepare the Standard solution and the Test solution.
to:
It meets the requirements of the test for Organic Impurities under Albuterol, except to read Albuterol Sulfate in place of Albuterol and to use water instead of methanol as the solvent to prepare the Standard solution and the Sample solution.

Change
Using the Injection as the Test solution, proceed as directed for Color and clarity under Isoproterenol Inhalation Solution.
to:
Standard solution—Transfer 2.0 mL of 0.100 N iodine VS to a 500-mL volumetric flask, dilute with water to volume, and mix.
Procedure—Visually examine a portion of the Injection (Test solution) in a suitable clear glass test tube against a white background: it is not pinkish and it contains no precipitate. If any yellow color is observed in the Test solution, concomitantly determine the absorbances of the Test solution and the Standard solution in 1-cm cells with a suitable spectrophotometer set at 460 nm: the absorbance of the Test solution does not exceed that of the Standard solution.

Change
Ammonium bicarbonate solution, Diluent, Solution A, Solution B, Mobile phase, Internal standard solution, and Chromatographic system—Proceed as directed in the Assay under Dimenhydrinate Tablets.
to:
Ammonium bicarbonate solution—Dissolve 4 g of ammonium bicarbonate in 250 mL of water.
Diluent—Dissolve 4 g of ammonium bicarbonate in 200 mL of water. Add 50 mL of methanol, and mix.
Solution A—Dissolve 0.8 g of ammonium bicarbonate in 800 mL of water. Add 200 mL of methanol, filter, and degas.
Solution B—Dissolve 0.8 g of ammonium bicarbonate in 150 mL of water. Add 850 mL of methanol, filter, and degas.
Mobile phase—Use variable mixtures of Solution A and Solution B as directed for Chromatographic system. Make adjustments if necessary (see System Suitability under Chromatography 〈621〉).
Internal standard solution—Prepare a solution in methanol containing 2.0 mg of 2-hydroxybenzyl alcohol per mL.
AND
Change
Standard solution—Prepare as directed for Standard preparation in the Assay under Dimenhydrinate Tablets.
to:
Standard solution—Accurately weigh about 50 mg of USP Dimenhydrinate RS, add about 5 mL of Ammonium bicarbonate solution and 20.0 mL of Internal standard solution, and mix. To 1 mL of this solution add about 9 mL of Diluent, and mix.
AND
Add
Chromatographic system (see Chromatography 〈621〉)—The liquid chromatograph is equipped with a 229-nm detector and a 4.6-mm × 25-cm column that contains packing L7. The flow rate is about 1.5 mL per minute. The chromatograph is programmed as follows.

Time (minutes), 0, 0–7.0, 7.0–7.1, 7.1–15, 15–15.1, 15.1–22.0
Solution A (%), 100, 100, 100→0, 0, 0→100, 100
Solution B (%), 0, 0, 0→100, 100, 100→0, 0
Elution, equilibration, isocratic, linear gradient, isocratic, linear gradient, isocratic

Chromatograph the Standard solution, and record the peak areas as directed for Procedure: the relative retention times are about 0.3 for 8-chlorotheophylline, 0.5 for the internal standard, and 1.0 for diphenhydramine; the resolution, R, between 8-chlorotheophylline and the internal standard is not less than 4.5; and the relative standard deviation for replicate injections is not more than 2.0%.

Line 5: Change
Potassium stock solution and Standard preparations—
to:
Standard stock solution and Standard solutions—
AND
Line 7 of Procedure: Change
for Procedure in the Assay under Potassium Chloride Oral Solution.
to:
for Instrumental conditions and Analysis in the Assay under Potassium Chloride Oral Solution.

In Test 2: Change
Determine the amount of isosorbide dinitrate (C₆H₉NO₆) dissolved by employing the following method.
to:
Determine the amount of isosorbide dinitrate (C₆H₈N₂O₈) dissolved by employing the following method.

Line 5: Change
Potassium stock solution—
to:
Standard stock solution—
AND
Line 7: Change
Prepare as directed for Standard preparations
to:
Prepare as directed for Standard solutions
AND
Line 7 of Procedure: Change
for Procedure in the Assay under Potassium Chloride Oral Solution.
to:
for Instrumental conditions and Analysis in the Assay under Potassium Chloride Oral Solution.

Line 1 of Mobile phase: Change
Prepare a filtered and degassed mixture of water, acetonitrile, ammonium acetate, glacial acetic acid, and triethylamine (1500:500:2:2:0.4). Make adjustments if necessary (see System Suitability under Chromatography <621>).
to:
Transfer 2 grams of ammonium acetate, 2 mL of glacial acetic acid, and 0.4 mL of triethylamine to a suitable flask containing 1500 mL of water and 500 mL of acetonitrile. Stir until all solids are dissolved and well mixed, then filter and degas.