Errata - English

Line 5 of paragraph 1 of Robust Design During Development: Change
lamellae (46,47)
to:
lamellae as discussed in Evaluation of the Inner Surface Durability of Glass Containers <1660> and by the FDA (45)
AND
Line 2 of paragraph 4 of Robust Design During Development: Change
(ICH)-relevant trials.
to:
(ICH)-relevant trials (46).

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
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 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 Application/4.: Change
proscribed
to:
prescribed
AND
Line 3 of Description of Polymers Contained in <661.1>/Polyethylenes: Change
Low-density polypropylene (LDPE)
to:
Low-density polyethylene (LDPE)
AND
Line 6 of Description of Polymers Contained in <661.1>/Polypropylene: Change
0.3% polypropylene
to:
0.3%. Polypropylene
AND
Line 3 of Description of Polymers Contained in <661.1>/Polyethylene Terephthalate and Polyethylene Terephthalate G: Change
1,4-cyclohexaemimethanol
to:
1,4-cyclohexanedimethanol

Line 1 of Vitamin A, Method 1/Sample solution: Change
Sample solution
to:
Sample stock solution
AND
Line 16 of Sample solution: Change
Dilute a 10-mL volume of this solution
to:
Sample solution: Dilute a 10-mL volume of the Sample stock solution
AND
Line 1 of Cholecalciferol or Ergocalciferol (Vitamin D), Method 1/Sample solution: Change
Proceed as directed for the Sample solution
to:
Proceed as directed for the Sample stock solution
AND
Line 1 of Vitamin E, Method 1/Sample solution: Change
Proceed as directed for the Sample solution
to:
Proceed as directed for the Sample stock solution
AND
Line 2 of Phytonadione, Method 1/Sample solution: Change
retained as specified in the directions for the Sample solution
to:
retained as specified in the directions for the Sample stock solution

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 1 of Sample solution: Change
Transfer 3.0 mL of the clear filtrate, reserved from the Assay, to a 100-mL volumetric flask.
to:
Sample stock solution: Dilute the clear filtrate, reserved from the Assay, with water to obtain a solution containing about 160 µg/mL of potassium citrate monohydrate.
Sample solution: Transfer 3.0 mL of the Sample stock solution to a 100-mL volumetric flask.

Line 1: Change
Buffer solution and Mobile phase—Prepare as directed in the Assay under Diluted Isosorbide Dinitrate.
to:
Buffer solution and Mobile phase—Prepare as directed in the Assay.
AND
Line 1 of Chromatographic system: Change
(see Chromatography <621>)—Proceed as directed in the Assay under Diluted Isosorbide Dinitrate.
to:
(see Chromatography <621>)—Proceed as directed in the Assay.

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 2 of USP Miconazole Related Compound C RS: Change
2-[(2,4-Dichlorobenzyl)oxy]-2-(2,4-dichlorophenyl)ethan-1-amine.
C₁₅H₁₃Cl₄NO 365.08
to:
2-[(2,4-Dichlorobenzyl)oxy]-2-(2,4-dichlorophenyl)ethan-1-amine hydrochloride.
C₁₅H₁₃Cl₄NO · HCl 401.53

Line 1 of Vitamin A, Method 1/Sample solution: Change
Sample solution
to:
Sample stock solution
AND
Line 23 of Vitamin A, Method 1/Sample solution: Change
Dilute a volume of this solution
to:
Sample solution: Dilute a volume of the Sample stock solution
AND
Line 2 of Cholecalciferol or Ergocalciferol (Vitamin D), Method 1/Sample solution:Change
prepared as directed for the Sample solution
to:
prepared as directed for the Sample stock solution
AND
Line 2 of Vitamin E, Method 1/Sample solution:Change
prepared as directed for the Sample solution
to:
prepared as directed for the Sample stock solution
AND
Line 2 of Phytonadione:Change
prepared as directed for the Sample solution
to:
prepared as directed for the Sample stock solution

Line 2 of USP Candesartan Cilexetil Related Compound D RS: Change
1-{[(Cyclohexyloxycarbonyloxy)carbonyl]oxy}ethyl 3-{[2’-(2-ethyl-2H-tetrazol-5-yl)biphenyl-4-yl]methyl}-2-oxo-2,3-dihydro-1H-benzimidazole-4-carboxylate.
to:
1-{[(Cyclohexyloxy)carbonyl]oxy}ethyl 3-({2’-(2-ethyl-2H-tetrazol-5-yl)-[1,1'-biphenyl]-4-yl}methyl)-2-oxo-2,3-dihydro-1H-benzimidazole-4-carboxylate.

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 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 2 of USP Doxepin Related Compound C RS: Change
(E,Z)-3-(Dibenzo[b,e]oxepin-11(6H-ylidene)-N-methyl-propoan-1-amine.
to:
(E,Z)-3-(Dibenzo[b,e]oxepin-11(6H)-ylidene)-N-methylpropan-1-amine hydrochloride.

Line 4 of USP Almotriptan Related Compound B RS: Change
C₁₅H₂₂N₃O₂S
to:
C₁₅H₂₁N₃O₂S
AND
Line 2 of USP Almotriptan Related Compound D RS: Change
1-[({3-[2-(Dimethylamino)ethyl]indol-5-yl}methyl)sulfonyl]pyrrolidine N-oxide.
C₁₇H₂₅N₃O₃S 351.46
to:
1-[({3-[2-(Dimethylamino)ethyl]indol-5-yl}methyl)sulfonyl]pyrrolidine N-oxide hydrochloride.
C₁₇H₂₅N₃O₃S · HCl 387.92

Change footnotes
^dEthyl 5-benzoyl-1-methylbenzimidazol-2-ylcarbamate.
^eMethyl 5-(4-toluoyl)-1-methylbenzimidazol-2-ylcarbamate.
to:
^dEthyl (5-benzoyl-1H-benzimidazol-2-yl)carbamate.
^eMethyl 5-(4-toluoyl)-1H-benzimidazol-2-ylcarbamate.

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 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 1 of Vitamin A, Method 1/Sample solution: Change
Sample solution
to:
Sample stock solution
AND
Line 16 of Sample solution: Change
Dilute a 10-mL volume of this solution
to:
Sample solution: Dilute a 10-mL volume of the Sample stock solution
AND
Line 2 of Cholecalciferol or Ergocalciferol (Vitamin D), Method 1/Sample solution: Change
prepared as directed for the Sample solution
to:
prepared as directed for the Sample stock solution
AND
Line 2 of Vitamin E, Method 1/Sample solution: Change
prepared as directed for the Sample solution
to:
prepared as directed for the Sample stock solution
AND
Line 2 of Phytonadione, Method 1/Sample solution: Change
prepared as directed for the Sample solution
to:
prepared as directed for the Sample stock solution