Errata - English

Line 1 of Sample solution: Change
1.1 µg/mL of sodium fluoride
to:
0.5 µg/mL of fluoride ion
AND
In the variable definition list in Analysis: Change
C_U = nominal concentration of sodium fluoride in the Sample solution (µg/mL)
to:
C_U = nominal concentration of fluoride ion in the Sample solution (µg/mL)

This erratum applies to the new USP-NF ONLINE platform only.
Line 1 of Standard stock solution 2: Change
0.1 mg/mL of in Diluent.
to:
0.1 mg/mL of USP Triamterene Related Compound A RS in Diluent.
AND
Line 1 of Standard stock solution 3: Change
0.1 mg/mL of USP Tranylcypromine Related Compound B RS in Diluent.
to:
0.1 mg/mL of USP Triamterene Related Compound B RS in Diluent.

Line 3 of A. Thin-Layer Chromatography/Presence of chicoric acid and absence of echinacoside/System suitability: Change
Standard solution B shows two major blue bands at about the middle of the chromatogram due to caftaric acid (lower R_F) and chlorogenic acid (higher R_F) that are clearly separated,
to:
Standard solution B shows two major blue bands at about the middle of the chromatogram due to caftaric acid (higher R_F) and chlorogenic acid (lower R_F) that are clearly separated,

In the second Calculate statement: Change
chloroindolinone and ziprasidone related compound F
to:
chloroindolinone, ziprasidone related compound F, and any individual unspecified impurity
AND
In the second variable definition list: Change
F = relative response factor for chloroindolinone or ziprasidone related compound F from Table 3
to:
F = relative response factor for chloroindolinone or ziprasidone related compound F or any individual unspecified impurity from Table 3

Line 1: Change
Proceed with Ophthalmic Suspension as directed in the Assay under Hydrocortisone Acetate Injectable Suspension.
to:
Standard preparation—Prepare as directed for Assay for Steroids <351>, Standard Preparation, using USP Hydrocortisone Acetate RS.
Assay preparation—Transfer to a separator an accurately measured volume of Ophthalmic Suspension, equivalent to about 50 mg of hydrocortisone acetate, and dilute with water to about 15 mL. Extract with four 25-mL portions of chloroform, filtering each portion through chloroform-washed cotton into a 250-mL volumetric flask. Add chloroform to volume, and mix. Pipet 10 mL of this solution into a 100-mL volumetric flask, add chloroform to volume, and mix. Pipet 10 mL of the resulting solution into a glass-stoppered, 50-mL conical flask, evaporate the chloroform on a steam bath just to dryness, cool, and dissolve the residue in 20.0 mL of alcohol.
Procedure—Proceed as directed for Assay for Steroids <351>, Procedure. Calculate the quantity, in mg, of hydrocortisone acetate (C₂₃H₃₂O₆) in each mL of Ophthalmic Suspension taken by the formula:
5(C/V)(A_U/A_S)
in which V is the volume, in mL, of Ophthalmic Suspension taken; and the other terms are defined therein.

Line 2 of USP Irinotecan Related Compound C RS: Change
(S)-9-[(1,4′-Bipiperidine)-1′-carbonyloxy]-4-methyl-11-ethyl-3,4,12,14-tetrahydro-4-hydroxy-3,14-dioxo-1H-pyrano[3′,4′:6,7]indolizino[1,2-b]quinoline hydrochloride.
to:
11-Ethyl-4-hydroxy-4-methyl-3,14-dioxo-3,4,12,14-tetrahydro-1H-pyrano[3′,4′:6,7]indolizino[1,2-b]quinolin-9-yl (1,4′-bipiperidine)-1′-carboxylate hydrochloride.

In the second variable definition in Analysis: Change
r_U = peak response of chloroindolinone or ziprasidone related compound F from the Sample solution
to:
r_U = peak response of chloroindolinone, ziprasidone related compound F, or any unspecified impurity from the Sample solution

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 3 of A. Thin-Layer Chromatography/Presence of chicoric acid and absence of echinacoside/System suitability: Change
Standard solution B shows two major blue bands at about the middle of the chromatogram due to caftaric acid (lower R_F) and chlorogenic acid (higher R_F) that are clearly separated,
to:
Standard solution B shows two major blue bands at about the middle of the chromatogram due to caftaric acid (higher R_F) and chlorogenic acid (lower R_F) that are clearly separated,

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.

Change
Test preparation: Into a 50-mL color-comparison tube place 10.0 mL of Solution S.
to:
Test preparation: Into a 50-mL color-comparison tube pipet 10.0 mL of Solution S and dilute with water to 25 mL. Using a pH meter or short-range pH indicator paper as external indicator, adjust with 1 N acetic acid or 6 N ammonium hydroxide to a pH of between 3.0 and 4.0, dilute with water to 40 mL, and mix.

Line 2 of USP Eszopiclone Related Compound A RS:
[Note—This material may be available in the free base or salt form.]
6-(5-Chloropyridin-2-yl)-7-oxo-6,7-dihydro-5H-pyrrolo[3,4-b]pyrazin-5-yl 4-methylpiperazine-1-carboxylate 4-oxide.
C₁₇H₁₇ClN₆O₄ 404.81
6-(5-Chloropyridin-2-yl)-7-oxo-6,7-dihydro-5H-pyrrolo[3,4-b]pyrazin-5-yl 4-methylpiperazine-1-carboxylate 4-oxide, 3-chlorobenzoic salt (1:1).
C₁₇H₁₇ClN₆O₄ · C₇H₅ClO 561.38
to:
[Note—This material may be available in the free base or salt form.]
6-(5-Chloropyridin-2-yl)-7-oxo-6,7-dihydro-5H-pyrrolo[3,4-b]pyrazin-5-yl 4-methylpiperazine-1-carboxylate 4-oxide.
C₁₇H₁₇ClN₆O₄ 404.81
6-(5-Chloropyridin-2-yl)-7-oxo-6,7-dihydro-5H-pyrrolo[3,4-b]pyrazin-5-yl 4-methylpiperazine-1-carboxylate 4-oxide, 3-chlorobenzoate salt (1:1).
C₁₇H₁₇ClN₆O₄ · C₇H₅ClO₂ 561.38

In Acid stage/Analysis/variable definition list: Change
V = volume of Medium, 750 mL
to:
V = volume of Acid stage medium, 750 mL
AND
In Buffer stage/Analysis/variable definition list: Change
V = volume of Medium, 1000 mL
to:
V = volume of Buffer stage medium, 1000 mL

Line 1 of Standard stock solution: Change
50 mg of USP Nifedipine RS in Diluent A and water (50:50)
to:
0.50 mg/mL of USP Nifedipine RS prepared as follows. Transfer a suitable amount of USP Nifedipine RS to an appropriate volumetric flask. Dissolve in 50% of the flask volume of Diluent A. Dilute with water to volume.
AND
Line 1 of Instrumental conditions/Analytical wavelength: Change
238 nm
to:
338 nm

Line 1 of Medium B: Change
Kreb's salt solution containing 0.3% (v/v) human serum albumen
to:
Krebs' salt solution containing 0.3% (v/v) human serum albumin
AND
Line 1 of Medium C: change
Kreb's salt solution containing 0.3% (v/v) human serum albumen
to:
Krebs' salt solution containing 0.3% (v/v) human serum albumin

(Note: This errata applies to the new USP-NF ONLINE platform only.)
Line 1 of System suitability solution: Change
0.1 mg/mL of USP Miconazole Nitrate RS and 6 µg/mL of USP Econazole Nitrate RS in Diluent.
to:
0.1 mg/mL of USP Miconazole Nitrate RS and 6 µg/mL of USP Miconazole Related Compound F RS in Diluent.

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.

In the second variable definition list: Change
C_S2 = concentration of USP Cholesterol RS in the Standard solution (mg/mL)
to:
C_S2 = concentration of USP Cholesterol RS in the System suitability solution (mg/mL)

Footnote e and f: Change
^e Methyl 7-chloro-6,7,8-trideoxy-6-[(2S,4R)-1-methyl-4-ethylpyrrolidine-2-carboxamido]-1-thio-L-threo-α-D-galacto-octopyranoside 3-phosphate.
^f Methyl 7-chloro-6,7,8-trideoxy-6-[(2S,4R)-1-methyl-4-propylpyrrolidine-2-carboxamido]-1-thio-D-threo-α-D-galacto-octopyranoside.
to:
^e Methyl 7-chloro-6,7,8-trideoxy-6-[(2S,4R)-1-methyl-4-propylpyrrolidine-2-carboxamido]-1-thio-L-threo-α-D-galacto-octopyranoside 3-phosphate.
^f Methyl 7-chloro-6,7,8-trideoxy-6-[(2S,4R)-1-methyl-4-propylpyrrolidine-2-carboxamido]-1-thio-L-threo-α-D-galacto-octopyranoside.

Line 2 of USP Eszopiclone Related Compound A RS:
[Note—This material may be available in the free base or salt form.]
6-(5-Chloropyridin-2-yl)-7-oxo-6,7-dihydro-5H-pyrrolo[3,4-b]pyrazin-5-yl 4-methylpiperazine-1-carboxylate 4-oxide.
C₁₇H₁₇ClN₆O₄ 404.81
6-(5-Chloropyridin-2-yl)-7-oxo-6,7-dihydro-5H-pyrrolo[3,4-b]pyrazin-5-yl 4-methylpiperazine-1-carboxylate 4-oxide, 3-chlorobenzoic salt (1:1).
C₁₇H₁₇ClN₆O₄ · C₇H₅ClO 561.38
to:
[Note – This material may be available in the free base or salt form.]
6-(5-Chloropyridin-2-yl)-7-oxo-6,7-dihydro-5H-pyrrolo[3,4-b]pyrazin-5-yl 4-methylpiperazine-1-carboxylate 4-oxide.
C₁₇H₁₇ClN₆O₄ 404.81
6-(5-Chloropyridin-2-yl)-7-oxo-6,7-dihydro-5H-pyrrolo[3,4-b]pyrazin-5-yl 4-methylpiperazine-1-carboxylate 4-oxide, 3-chlorobenzoate salt (1:1).
C₁₇H₁₇ClN₆O₄ · C₇H₅ClO₂ 561.38