Errata - English

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.

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.

In the equation in Standardization: Change
N = mg K₂Cr₂O₇/49.04 x mL Na₂S₂O₃
to:
M = mg K₂Cr₂O₇/49.04 x mL Na₂S₂O₃

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.

Line 2 of USP Salmeterol Related Compound H RS: Change
1-Hydroxy-4-[2-hydroxy-5-(1-hydroxy-2-{[6-(4-phenylbutoxy)hexyl]amino}ethyl)benzyl]-2-naphthoic acid.
C₃₆H₄₃NO₆ 585.73
to:
1-Hydroxy-4-[2-hydroxy-5-(1-hydroxy-2-{[6-(4-phenylbutoxy)hexyl]amino}ethyl)benzyl]-2-naphthoic acid, monohydrate.
C₃₆H₄₃NO₆ · H₂O 603.76

Line 2 of USP Salmeterol Related Compound H RS: Change
1-Hydroxy-4-[2-hydroxy-5-(1-hydroxy-2-{[6-(4-phenylbutoxy)hexyl]amino}ethyl)benzyl]-2-naphthoic acid.
C₃₆H₄₃NO₆ 585.73
to:
1-Hydroxy-4-[2-hydroxy-5-(1-hydroxy-2-{[6-(4-phenylbutoxy)hexyl]amino}ethyl)benzyl]-2-naphthoic acid, monohydrate.
C₃₆H₄₃NO₆ · H₂O 603.76

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.

Footnote m: Change
(2S,5R,6R)-Ethyl 6-((R)-2-{(2S,5R,6R)-6-[(R)-2-(4-ethyl-2,3-dioxopiperazine-1-carboxamido)-2-phenylacetamido]-3,3-dimethyl-7-oxo-4-thia-1-azabicyclo[3.2.0]heptane-2-carboxamido}-2-phenylacetamido)-3,3-dimethyl-7-oxo-4-thia-1-azabicyclo[3.2.0]heptane-2-carboxylate.
to:
2-(((3-Acetyl-4-(ethoxycarbonyl)-5,5-dimethylthiazolidin-2-yl)methyl)amino)-2-oxo-1-phenylethyl 6-(2-(4-ethyl-2,3-dioxopiperazine-1-carboxamido)-2-phenylacetamido)-3,3-dimethyl-7-oxo-4-thia-1-azabicyclo[3.2.0]heptane-2-carboxylate.

Line 1 of Sample solution: Change
25 mg/mL of Norepinephrine Bitartrate in glacial acetic acid. If necessary warm slightly to effect solution.
to:
Dissolve 500 mg of Norepinephrine Bitartrate in 20 mL of glacial acetic acid, warming slightly if necessary to effect solution.

Line 5 of A. Thin-Layer Chromatography/Presence of echinacoside and absence of dicaffeoylquinic acid/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,
AND
Lines 3 and 6 of C.: Change
Standard solution B,
to:
Standard solution C,
AND
Change
Standard solution C)
to:
Standard solution D)

Line 2 of USP Eszopiclone Related Compound A RS: Change
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
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-chlorobenzoic salt (1:1).
C₁₇H₁₇ClN₆O₄ · C₇H₅ClO 561.38

Line 3 of Standard solution A: Change
lead acetate,
to:
lead acetate TS,
AND
Line 11 of Analysis: Change
Locate the two prominent bands from Standard solution A corresponding in R_F value to the two bands from Standard solution B.
to:
Locate the prominent bands from Standard solution A corresponding in R_F value to the band from Standard solution B.

Line 5 of A. Thin-Layer Chromatography/Presence of echinacoside and absence of dicaffeoylquinic acid/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,
AND
Lines 3 and 6 of C.: Change
Standard solution B,
to:
Standard solution C,
AND
Change
Standard solution C)
to:
Standard solution D)

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 4 of A. HPTLC for Articles of Botanical Origin <203>/For Capsules containing Echinacea angustifolia powder prepared from dried rhizome and roots/System suitability: Change
Standard solution B shows two major blue bands at about the middle section 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 section due to caftaric acid (higher R_F) and chlorogenic acid (lower R_F) that are clearly separated,

Line 2 of USP Timolol Related Compound A RS: Change
(R)-1-(tert-Butylamino)-3-(4-morpholino-1,2,5-thiadiazol-3-yloxy)propan-2-ol.
C₁₃H₂₄N₄O₃S 316.42
to:
(R)-1-(tert-Butylamino)-3-(4-morpholino-1,2,5-thiadiazol-3-yloxy)propan-2-ol maleate.
C₁₃H₂₄N₄O₃S · C₄H₄O₄ 432.49
AND
Line 2 of USP Timolol Related Compound C RS: Change
N-(tert-Butyl)-2,3-bis(4-morpholino-1,2,5-thiadiazol-3-yloxy)propan-1-amine.
C₁₉H₃₁N₇O₄S₂ 485.19
to:
N-(tert-Butyl)-2,3-bis(4-morpholino-1,2,5-thiadiazol-3-yloxy)propan-1-amine maleate.
C₁₉H₃₁N₇O₄S₂ ∙ C₄H₄O₄ 601.69
AND
Line 3 of USP Timolol Related Compound D RS: Change
C₆H₉N₇O₄S
to:
C₆H₉N₃O₂S
AND
Line 2 of USP Timolol Related Compound E RS: Change
(S)-3-(tert-Butylamino)-1-(4-morpholino-1,2,5-thiadiazol-3-yloxy)propan-2-yl hydrogen maleate.
C₁₇H₂₆N₄O₆S 414.48
to:
(S,Z)-4-({1-(tert-Butylamino)-3-[(4-morpholino-1,2,5-thiadiazol-3-yl)oxy]propan-2-yl}oxy)-4-oxobut-2-enoic acid maleate salt (1:1)
C₁₇H₂₆N₄O₆S ∙ C₄H₄O₄ 530.55

Line 2 of USP Eszopiclone Related Compound A RS: Change
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
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-chlorobenzoic salt (1:1).
C₁₇H₁₇ClN₆O₄ · C₇H₅ClO 561.38

Line 5 of A. Thin-Layer Chromatography/Presence of echinacoside and dicaffeoylquinic acid/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,
AND
Line 3 of C.: Change
Standard solution B,
to:
Standard solution C,

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) 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 4 of A. HPTLC for Articles of Botanical Origin <203>/For Capsules containing Echinacea angustifolia Dry Extract/System suitability: Change
Standard solution B shows two major blue bands at about the middle section 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 section due to caftaric acid (higher R_F) and chlorogenic acid (lower R_F) that are clearly separated,

Line 5 of A. Thin-Layer Chromatography/Presence of echinacoside and absence of dicaffeoylquinic acid/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,
AND
Lines 3 and 6 of C.: Change
Standard solution B,
to:
Standard solution C,
AND
Change
Standard solution C)
to:
Standard solution D)

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,