usp-nf redesign monographs
TRANSCRIPT
USP-NF Redesign MonographsAcarbose Acetaminophen and Pseudoephedrine Hydrochloride Tablets
Acebutolol Hydrochloride Acetazolamide
Acepromazine Maleate Acetazolamide Oral Suspension
Acepromazine Maleate Injection Acetazolamide Tablets
Acepromazine Maleate Tablets Glacial Acetic Acid
Acetaminophen Acetic Acid Irrigation
Acetaminophen Oral Solution Acetohexamide
Acetaminophen Suppositories Acetohydroxamic Acid
Acetaminophen Tablets Acetylcholine Chloride
Acetaminophen and Aspirin Tablets Acetylcysteine
Acetaminophen, Aspirin, and Caffeine Tablets Acetylcysteine Solution
Acetaminophen and Caffeine Tablets Acetylcysteine and Isoproterenol Hydrochloride Inhalation Solution
Capsules Containing at Least Three of the Following—Acet- aminophen and Salts of Chlorpheniramine, Dex- Acitretin tromethorphan, and Phenylpropanolamine
Acitretin Capsules Oral Solution Containing at Least Three of the Following—
AcyclovirAcetaminophen and Salts of Chlorpheniramine, Dex- tromethorphan, and Phenylpropanolamine Acyclovir Capsules Tablets Containing at Least Three of the Following—Acet- Acyclovir for Injection aminophen and Salts of Chlorpheniramine, Dex- tromethorphan, and Phenylpropanolamine Acyclovir Ointment
Capsules Containing at Least Three of the Following—Acet- Acyclovir Oral Suspension aminophen and Salts of Chlorpheniramine, Dex-
Acyclovir Tabletstromethorphan, and Pseudoephedrine AdenineOral Powder Containing at Least Three of the Following—
Acetaminophen and Salts of Chlorpheniramine, Dex- Adenosine tromethorphan, and Pseudoephedrine
Adenosine Injection Oral Solution Containing at Least Three of the Following— Acetaminophen and Salts of Chlorpheniramine, Dex- Medical Air tromethorphan, and Pseudoephedrine
Alanine Tablets Containing at Least Three of the Following—Acet-
Albendazoleaminophen and Salts of Chlorpheniramine, Dex- tromethorphan, and Pseudoephedrine Albendazole Oral Suspension Acetaminophen, Chlorpheniramine Maleate, and Dex- Albendazole Tablets tromethorphan Hydrobromide Tablets
Albumin Human Acetaminophen and Codeine Phosphate Capsules
Albuterol Acetaminophen and Codeine Phosphate Oral Solution
Albuterol Sulfate Acetaminophen and Codeine Phosphate Oral Suspension
Albuterol Tablets Acetaminophen and Codeine Phosphate Tablets
Alclometasone Dipropionate Acetaminophen, Dextromethorphan Hydrobromide, Doxyl- amine Succinate, and Pseudoephedrine Hydrochloride Oral Alclometasone Dipropionate Cream Solution
Alclometasone Dipropionate Ointment Acetaminophen and Diphenhydramine Citrate Tablets
Alcohol Acetaminophen, Diphenhydramine Hydrochloride, and
Dehydrated AlcoholPseudoephedrine Hydrochloride Tablets
Copyright 2008 The United States Pharmacopeial Convention. All Rights Reserved. For Discussion Purposes Only — Not for Dissemination
2 / MONOGRAPH LIST USP 32
Dehydrated Alcohol Injection Aluminum Chloride
Rubbing Alcohol Aluminum Chlorohydrate
Alendronate Sodium Aluminum Chlorohydrex Polyethylene Glycol
Alendronate Sodium Tablets Aluminum Chlorohydrex Propylene Glycol
Alfentanil Hydrochloride Aluminum Dichlorohydrate
Alfuzosin Hydrochloride Aluminum Dichlorohydrex Polyethylene Glycol
Allantoin Aluminum Dichlorohydrex Propylene Glycol
Allopurinol Aluminum Hydroxide Gel
Aloe Aluminum Phosphate Gel
Alprostadil Aluminum Sesquichlorohydrex Propylene Glycol
Alprostadil Injection Aluminum Subacetate Topical Solution
Alteplase Aluminum Sulfate
Alteplase for Injection Aluminum Sulfate and Calcium Acetate for Topical Solution
Altretamine Aluminum Sulfate and Calcium Acetate Tablets for Topical Solution
Altretamine Capsules Aluminum Zirconium Octachlorohydrate
Ammonium Alum Aluminum Zirconium Octachlorohydrate Solution
Potassium Alum Aluminum Zirconium Octachlorohydrex Gly
Alumina and Magnesia Oral Suspension Aluminum Zirconium Octachlorohydrex Gly Solution
Alumina and Magnesia Tablets Aluminum Zirconium Pentachlorohydrate
Alumina, Magnesia, and Calcium Carbonate Oral Suspension Aluminum Zirconium Pentachlorohydrate Solution
Alumina, Magnesia, and Calcium Carbonate Tablets Aluminum Zirconium Pentachlorohydrex Gly
Alumina, Magnesia, and Calcium Carbonate Chewable Tablets Aluminum Zirconium Pentachlorohydrex Gly Solution
Alumina, Magnesia, Calcium Carbonate, and Simethicone Aluminum Zirconium Tetrachlorohydrate Tablets
Aluminum Zirconium Tetrachlorohydrate Solution Alumina, Magnesia, Calcium Carbonate, and Simethicone
Aluminum Zirconium Tetrachlorohydrex GlyChewable Tablets Aluminum Zirconium Tetrachlorohydrex Gly SolutionAlumina, Magnesia, and Simethicone Oral Suspension Aluminum Zirconium TrichlorohydrateAlumina, Magnesia, and Simethicone Tablets Aluminum Zirconium Trichlorohydrate SolutionAlumina, Magnesia, and Simethicone Chewable Tablets Aluminum Zirconium Trichlorohydrex GlyAlumina and Magnesium Carbonate Oral Suspension Aluminum Zirconium Trichlorohydrex Gly SolutionAlumina and Magnesium Carbonate Tablets Amantadine HydrochlorideAlumina, Magnesium Carbonate, and Magnesium Oxide
Tablets Amantadine Hydrochloride Capsules Alumina and Magnesium Trisilicate Oral Suspension Amantadine Hydrochloride Oral Solution Alumina and Magnesium Trisilicate Tablets Amcinonide Aluminum Acetate Topical Solution
Copyright 2008 The United States Pharmacopeial Convention. All Rights Reserved. For Discussion Purposes Only — Not for Dissemination
USP 32 MONOGRAPH LIST / 3
Amcinonide Cream Amitriptyline Hydrochloride
Amifostine Amitriptyline Hydrochloride Tablets
Amikacin Aromatic Ammonia Spirit
Amikacin Sulfate Ammonium Chloride
Amiloride Hydrochloride and Hydrochlorothiazide Tablets Ferric Ammonium Citrate for Oral Solution
Amiloxate Ammonium Molybdate
Aminobenzoate Potassium for Oral Solution Amobarbital Sodium for Injection
Aminobenzoate Potassium Tablets Amodiaquine
Aminobenzoate Sodium Amodiaquine Hydrochloride
Aminobenzoic Acid Gel Amoxapine
Aminocaproic Acid Amoxicillin
Aminocaproic Acid Oral Solution Amoxicillin Capsules
Aminocaproic Acid Tablets Amoxicillin Intramammary Infusion
Aminoglutethimide Amoxicillin for Injectable Suspension
Aminoglutethimide Tablets Amoxicillin Oral Suspension
Aminohippurate Sodium Injection Amoxicillin for Oral Suspension
Aminohippuric Acid Amoxicillin Tablets
Aminopentamide Sulfate Injection Amoxicillin and Clavulanate Potassium for Oral Suspension
Aminopentamide Sulfate Tablets Amoxicillin and Clavulanate Potassium Tablets
Aminophylline Amphetamine Sulfate
Aminophylline Rectal Solution Amphotericin B Cream
Aminophylline Suppositories Amphotericin B for Injection
Aminophylline Tablets Amphotericin B Lotion
Aminophylline Delayed-Release Tablets Amphotericin B Ointment
Aminosalicylate Sodium Ampicillin
Aminosalicylic Acid Ampicillin Capsules
Amitraz Ampicillin Soluble Powder
Copyright 2008 The United States Pharmacopeial Convention. All Rights Reserved. For Discussion Purposes Only — Not for Dissemination
4 / MONOGRAPH LIST USP 32
Ampicillin for Oral Suspension Arginine Hydrochloride
Ampicillin Tablets Arginine Hydrochloride Injection
Ampicillin and Probenecid for Oral Suspension Arsanilic Acid
Ampicillin Sodium Ascorbic Acid
Amprolium Ascorbic Acid Oral Solution
Amprolium Soluble Powder Ascorbic Acid Tablets
Amprolium Oral Solution Aspartic Acid
Amyl Nitrite Aspirin
Anileridine Aspirin Capsules
Anileridine Hydrochloride Aspirin Suppositories
Anthralin Aspirin Delayed-Release Tablets
Anthralin Ointment Aspirin Extended-Release Tablets
Anthrax Vaccine Adsorbed Aspirin, Alumina, and Magnesia Tablets
Anticoagulant Citrate Dextrose Solution Aspirin, Alumina, and Magnesium Oxide Tablets
Anticoagulant Citrate Phosphate Dextrose Solution Aspirin, Caffeine, and Dihydrocodeine Bitartrate Capsules
Anticoagulant Citrate Phosphate Dextrose Adenine Solution Aspirin and Codeine Phosphate Tablets
Anticoagulant Heparin Solution Aspirin, Codeine Phosphate, Alumina, and Magnesia Tablets
Anticoagulant Sodium Citrate Solution Astemizole
Antihemophilic Factor Astemizole Tablets
Cryoprecipitated Antihemophilic Factor Atenolol
Antimony Sodium Tartrate Atenolol Oral Solution
Antipyrine Atenolol Tablets
Antipyrine, Benzocaine, and Phenylephrine Hydrochloride Atovaquone Otic Solution
Atovaquone Oral Suspension Antithrombin III Human
Atracurium Besylate Antivenin (Crotalidae) Polyvalent
Atracurium Besylate Injection Antivenin (Latrodectus mactans)
Atropine Antivenin (Micrurus fulvius)
Atropine Sulfate Apomorphine Hydrochloride
Atropine Sulfate Ophthalmic Solution Apraclonidine Ophthalmic Solution
Atropine Sulfate Tablets Aprotinin
Activated Attapulgite Aprotinin Injection
Colloidal Activated Attapulgite Arginine
Copyright 2008 The United States Pharmacopeial Convention. All Rights Reserved. For Discussion Purposes Only — Not for Dissemination
USP 32 MONOGRAPH LIST / 5
Aurothioglucose Injectable Suspension Azathioprine Tablets
Avobenzone Azathioprine Sodium for Injection
Azaperone Azithromycin
Azatadine Maleate Tablets Aztreonam
Copyright 2008 The United States Pharmacopeial Convention. All Rights Reserved. For Discussion Purposes Only — Not for Dissemination
(Comment on this Monograph)
132270
AnalysisAcarbose Samples: Standard solution and Sample solutionid=m115=Acarbose=A- Calculate the percentage of C25H43NO18 in the portion ofMonos.pdf) Acarbose taken:
Result = (rU/rS) × (CS/CU) × 100
rU = peak response from the Sample solution rS = peak response from the Standard solution CS = concentration of USP Acarbose RS in the
Standard solution (mg/mL) CU = concentration of the Sample solution (mg/mL)C25H43NO18 645.60
Acceptance criteria: 95.0%–102.0%D-Glucose, O-4,6-dideoxy-4-[[[1S-(1α,4α,5β,6α)]-4,5,6- trihydroxy-3-(hydroxymethyl)-2-cyclohexen-1-yl]amino]-α-D- IMPURITIES glucopyranosyl-(1→4)-O-α-D-glucopyranosyl-(1→4)-; Inorganic Impurities
O-4,6-Dideoxy-4-[[(1S,4R,5S,6S)-4,5,6-trihydroxy-3- • RESIDUE ON IGNITION ⟨281⟩: NMT 0.2%, determined on 1.0 g (hydroxymethyl)-2-cyclohexen-1-yl]amino]-α-D- • HEAVY METALS, Method II ⟨231⟩: NMT 20 ppm glucopyranosyl-(1→4)-O-α-D-glucopyranosyl-(1→4)-D- Organic Impurities glucose [56180-94-0]. • PROCEDURE
Mobile phase, System suitability solution, andDEFINITION Chromatographic system: Proceed as directed in theAcarbose is produced by certain strains of Actinoplanes Assay.utahensis. It contains NLT 95.0% and NMT 102.0% of
Sample stock solution: Use the Sample solution, asC25H43NO18, calculated on the anhydrous basis. directed in the Assay.
Sample solution: Sample stock solution and water (1:99)IDENTIFICATION Analysis• A. INFRARED ABSORPTION ⟨197K⟩ Samples: Sample stock solution and Sample solution• B. The retention time of the Sample solution corresponds to Calculate the percentage of each impurity in the portionthat of the Standard solution, as obtained in the Assay. of Acarbose taken:
ASSAY Result = (ri/ra) × RRF × 100• PROCEDURE
Solution A: 0.6 mg/mL of monobasic potassium phosphate ri = peak response for each impurityand 0.35 mg/mL of dibasic sodium phosphate ra = response of the main acarbose peak in theMobile phase: Acetonitrile and Solution A (3:1)
chromatogram of the Sample solutionSystem suitability solution: Reconstitute a vial of USP RRF = relative response factor for each impurity, asAcarbose System Suitability Mixture RS in 1 mL of water.
listed in the Impurity TableStandard solution: Reconstitute a vial of USP Acarbose RS Acceptance criteriain 5.0 mL of water. Individual impurities: See Impurity Table.Sample solution: 20 mg/mL of Acarbose in water Total impurities: NMT 3.0%Chromatographic system
(See Chromatography ⟨621⟩, System Suitability.) Mode: LC Impurity Table Detector: UV 210 nm
Relative Relative AcceptanceColumn: 4-mm × 25-cm; packing L8 Retention Response Criteria,Temperature: 35°
Name Time Factor NMT (%)Flow rate: 2 mL/min Impurity Aa 0.9 1 0.6Injection size: 10 µL
System suitability Impurity Bb 0.8 1.6 0.5 Sample: System suitability solution
Impurity Cc 1.2 1 1.5[NOTE—Identify the acarbose peak and the peaks due to Impurity Dd 0.5 1.33 1.0the impurities listed in the Impurity Table.]
Suitability requirements Impurity Ee 1.7 0.8 0.2 Height to valley ratio: NLT 1.2 for the impurity A peak,
Impurity Ff 1.9 0.8 0.3and the valley between the impurity A peak and the Impurity Gg 2.2 0.8 0.3acarbose peak
[NOTE—The chromatogram obtained is similar to the Impurity Hh 0.6 1 0.2 chromatogram supplied with USP Acarbose System Suitability Mixture RS.]
Copyright 2008 The United States Pharmacopeial Convention. All Rights Reserved. For Discussion Purposes Only — Not for Dissemination
Impurity Table (continued) USP Acarbose System Suitability Mixture RS
Relative Relative Acceptance Retention Response Criteria,
Name Time Factor NMT (%) Acebutolol Hydrochloride Any individual — — 0.2 id=m125=Acebutolol unknown impurity Hydrochloride=A-Monos.pdf)
aO-4,6-Dideoxy-4-[[(1S,4R,5S,6S)-4,5,6-trihydroxy-3- (hydroxymethyl)cyclohex-2-enyl]amino]-α-D-glucopyranosyl-(1→4)-O-α-D- glucopyranosyl-(1→4)-D-arabino-hex-2-ulopyranose. b(1R,4R,5S,6R)-4,5,6-Trihydroxy-2-(hydroxymethyl)cyclohex-2-enyl 4-O- [4,6-dideoxy-4-[[(1S,4R,5S,6S)-4,5,6-trihydroxy-3- (hydroxymethyl)cyclohex-2-enyl]amino]-α-D-glucopyranosyl]-α-D- glucopyranoside.
Standard solution: 0.14 mg/mL of USP Acebutolol Hydrochloride RS
SPECIFIC TESTS Sample solution: 0.14 mg/mL of Acebutolol Hydrochloride • OPTICAL ROTATION, Specific Rotation ⟨781S⟩: +168° to +183° Chromatographic system
Sample solution: 10 mg/mL (See Chromatography ⟨621⟩, System Suitability.) • PH ⟨791⟩: 5.5–7.5, in a solution containing 50 mg/mL • WATER DETERMINATION, Method Ic ⟨921⟩: NMT 4.0%
ADDITIONAL REQUIREMENTS • PACKAGING AND STORAGE: Preserve in tight containers. • USP REFERENCE STANDARDS ⟨11⟩
USP Acarbose RS
Copyright 2008 The United States Pharmacopeial Convention. All Rights Reserved. For Discussion Purposes Only — Not for Dissemination
USP 32 Official Monographs / Acebutolol 3
Mode: LC ADDITIONAL REQUIREMENTS Detector: UV 254 nm • PACKAGING AND STORAGE: Preserve in tight containers, and Column: 3.9-mm × 30-cm; packing L1 store at controlled room temperature. Flow rate: 2 mL/min • USP REFERENCE STANDARDS ⟨11⟩ Injection size: 10 µL USP Acebutolol Hydrochloride RS
System suitability Sample: Standard solution Suitability requirements Acebutolol Hydrochloride CapsulesColumn efficiency: NLT 1500 theoretical plates Tailing factor: NMT 2.5 id=m127=Acebutolol Relative standard deviation: NMT 2.0% Hydrochloride Capsules=A-Monos.pdf)
Analysis DEFINITIONSamples: Standard solution and Sample solution Acebutolol Hydrochloride Capsules contain the equivalent ofCalculate the percentage of C18H28N2O4 · HCl in the NLT 90.0% and NMT 110.0% of the labeled amount ofAcebutolol Hydrochloride taken: acebutolol (C18H28N2O4).
Result = (rU/rS) × (CS/CU) × 100 IDENTIFICATION • The retention time of the Sample solution corresponds to thatrU = peak response from the Sample solution
of the Standard solution, as obtained in the Assay.rS = peak response from the Standard solution CS = concentration of USP Acebutolol Hydrochloride
ASSAYRS in the Standard solution (mg/mL) • PROCEDURECU = concentration of the Sample solution (mg/mL) Solution A: Dissolve 2.4 g of sodium 1-decanesulfonate inAcceptance criteria: 98.0%–102.0% 1000 mL of water. Adjust with glacial acetic acid to a pH of 3.5.IMPURITIES
Mobile phase: Methanol and Solution A (3:2)Inorganic Impurities Standard solution: 0.22 mg/mL of USP Acebutolol• RESIDUE ON IGNITION ⟨281⟩: NMT 0.1% Hydrochloride RS in methanol• HEAVY METALS, Method II ⟨231⟩: NMT 20 ppm [NOTE—This is equivalent to 0.2 mg/mL of acebutolol.]Organic Impurities
Sample stock solution: Weigh and mix, as completely as• PROCEDURE possible, the contents of NLT 20 Capsules. Transfer a portionStandard solution: 1.0 mg/mL of USP Acebutolol of the powder, equivalent to 200 mg of acebutolol, to aHydrochloride RS in methanol 200-mL volumetric flask. Add 180 mL of methanol, and stirReference solution A: Dilute 3.0 mL of the Standard by mechanical means for 30 min. Dilute with methanol tosolution with methanol to 100 mL. volume.Reference solution B: Dilute 5.0 mL of the Standard
Sample solution: Dilute 5.0 mL of the Sample stock solutionsolution with methanol to 100 mL. with methanol to 25 mL.Sample solution A: 10 mg/mL of Acebutolol
Chromatographic systemHydrochloride in methanol (See Chromatography ⟨621⟩, System Suitability.)Sample solution B: Sample solution A and methanol (1:9) Mode: LCDeveloping solvent system: Butyl alcohol, glacial acetic Detector: UV 254 nmacid, and water (4:1:5) Column: 3.9-mm × 15-cm; 5-µm packing L1Chromatographic system Flow rate: 1 mL/min(See Chromatography ⟨621⟩, Thin-Layer Chromatography.) Injection size: 20 µLMode: TLC
System suitabilityAdsorbent: 0.25-mm layer of chromatographic silica gel Sample: Standard solutionmixture Suitability requirementsApplication volume: 20 µL Tailing factor: NMT 1.5Analysis Relative standard deviation: NMT 2.0%Samples: Standard solution, Reference solution A, Reference
Analysissolution B, Sample solution A, and Sample solution B Samples: Standard solution and Sample solutionProceed as directed in the chapter. Develop the Calculate the percentage of C18H28N2O4 in the Capsuleschromatogram in the Developing solvent system until the taken:solvent front has moved three-fourths the length of the
plate. Examine the plate under short-wavelength UV Result = (rU/rS) × (CS/CU) × (Mr1/Mr2) × 100light.
Acceptance criteria: The chromatograms from Sample rU = peak response from the Sample solutionsolution B and the Standard solution show principal spots at rS = peak response from the Standard solutionthe same RF value. No secondary spot from Sample solution CS = concentration of USP Acebutolol HydrochlorideA, excluding the area at the point of application, is more
RS in the Standard solution (mg/mL)intense than the principal spot of Reference solution A CU = nominal concentration of the Sample solution(0.3%); NMT two secondary spots from Sample solution A
(mg/mL)are more intense than the principal spot of Reference Mr1 = molecular weight of acebutolol, 336.44solution B (0.1%); and the total of all impurities detected in Mr2 = molecular weight of acebutolol hydrochloride,the chromatogram of Sample solution A is NMT 0.5%.
372.89 SPECIFIC TESTS • MELTING RANGE OR TEMPERATURE ⟨741⟩: 140°–144° • PH ⟨791⟩: 4.5–7.0, in a solution (1 in 100) • LOSS ON DRYING ⟨731⟩: Dry it at 105° for 3 h: it loses NMT
1.0% of its weight
Copyright 2008 The United States Pharmacopeial Convention. All Rights Reserved. For Discussion Purposes Only — Not for Dissemination
4 Acebutolol / Official Monographs USP 32
Acceptance criteria: 90.0%–110.0% rS = peak response from the Standard solution CS = concentration of USP Acebutolol Hydrochloride
PERFORMANCE TESTS RS in the Standard solution (µg/mL) • DISSOLUTION ⟨711⟩ CU = nominal concentration of the Sample solution
Medium: Water; 900 mL (µg/mL) Apparatus 2: 50 rpm Mr1 = molecular weight of acebutolol, 336.44 Time: 30 min Mr2 = molecular weight of acebutolol hydrochloride, Sample solution: Sample per Dissolution ⟨711⟩. 372.89 Standard solution: USP Acebutolol Hydrochloride RS in Test 2 Medium Solution A: Prepare as directed in the Assay.
Spectrometric conditions Mobile phase: Methanol and Solution A (1:1) Mode: UV Standard solution: Transfer 30 mg of USP Acebutolol Analytical wavelength: 232 nm Hydrochloride RS to a 50-mL volumetric flask. Add 12 mL Analysis: Determine the amount of C18H28N2O4 dissolved of methanol, swirl to dissolve, and dilute with Mobile by employing the UV absorption on filtered portions of the phase to volume. Dilute a volume of this stock solution Sample solution in comparison with a Standard solution in with Mobile phase to obtain a concentration of 1.4 µg/mL the same Medium. of USP Acebutolol Hydrochloride RS.
Tolerances: NLT 80% (Q) of the labeled amount of Sample solution: Transfer a portion of the contents of 20 C18H28N2O4 is dissolved. opened Capsules, equivalent to 250 mg of acebutolol, to
• UNIFORMITY OF DOSAGE UNITS ⟨905⟩: Meet the requirements a 100-mL volumetric flask, add 25 mL of methanol, and shake by mechanical means for 15 min. Dilute with MobileIMPURITIES phase to volume. Centrifuge a portion of this solution,Organic Impurities and transfer 10.0 mL of the clear supernatant to a 100-mL• PROCEDURE volumetric flask. Dilute with Mobile phase to volume.Test 1 Chromatographic systemSolution A: Prepare as directed in the Assay. (See Chromatography ⟨621⟩, System Suitability.)Mobile phase: Methanol and Solution A (44:56) Mode: LCDiluent: Methanol and Solution A (1:1) Detector: UV 240 nmStandard solution: Transfer 30 mg of USP Acebutolol Column: 3.9 mm × 15 cm; 4-µm packing L1Hydrochloride RS to a 50-mL volumetric flask. Add 12 mL Flow rate: 1 mL/minof methanol, swirl to dissolve, and dilute with Diluent to Injection size: 70 µLvolume. Dilute a volume of this solution with Diluent to System suitabilityobtain a concentration of 1.4 µg/mL of USP Acebutolol Sample: Standard solutionHydrochloride RS. Suitability requirementsSample solution: Transfer a portion of the contents of 20 Relative standard deviation: NMT 6.0%opened Capsules, equivalent to 250 mg of acebutolol, to Analysisa 100-mL volumetric flask, add 25 mL of methanol, and Samples: Mobile phase, Standard solution, and Sampleshake by mechanical means for 15 min. Dilute with solutionDiluent to volume. Centrifuge a portion of this solution, Calculate the percentage of each impurity eluting afterand transfer 10.0 mL of the clear supernatant to a 100-mL the acebutolol peak in the portion of Capsules taken:volumetric flask. Dilute with Diluent to volume.
Chromatographic system Result = (rU/rS) × (CS/CU) × (Mr1/Mr2) × 100 (See Chromatography ⟨621⟩, System Suitability.) Mode: LC rU = peak response for any individual impurity from Detector: UV 240 nm the Sample solution Column: 3.9-mm ×15-cm; 4-µm packing L1 rS = peak response from the Standard solution Flow rate: 1 mL/min CS = concentration of USP Acebutolol Hydrochloride Injection size: 35 µL RS in the Standard solution (µg/mL)
System suitability CU = nominal concentration of the Sample solution Sample: Standard solution (µg/mL) Suitability requirements Mr1 = molecular weight of acebutolol, 336.44 Relative standard deviation: NMT 6.0% Mr2 = molecular weight of acebutolol hydrochloride,
Analysis 372.89 Samples: Diluent, Standard solution, and Sample solution Acceptance criteria
[NOTE—Record the chromatograms for two times the Test 1: NMT 0.5% of any individual impurity retention time of acebutolol, and measure the Test 2: NMT 0.5% of any individual impurity responses for all the peaks, disregarding any peaks Sum of impurities found in Test 1 and Test 2: NMT corresponding to those obtained from the Diluent.] 1.0%
Calculate the percentage of each impurity eluting prior to the acebutolol peak in the portion of Capsules taken: ADDITIONAL REQUIREMENTS
• PACKAGING AND STORAGE: Preserve in tight containers, and Result = (rU/rS) × (CS/CU) × (Mr1/Mr2) × 100 store at controlled room temperature.
• USP REFERENCE STANDARDS ⟨11⟩ rU = peak response for any individual impurity from USP Acebutolol Hydrochloride RS
the Sample solution
Copyright 2008 The United States Pharmacopeial Convention. All Rights Reserved. For Discussion Purposes Only — Not for Dissemination
(Comment on this Monograph)
(Comment on this Monograph)
Acceptance criteria: 98.0%–101.0%Acepromazine Maleate id=m134=Acepromazine IMPURITIES
Maleate=A-Monos.pdf) Inorganic Impurities • RESIDUE ON IGNITION ⟨281⟩: NMT 0.2% Organic Impurities • PROCEDURE
[NOTE—Conduct this test without exposure to daylight, and with the minimum necessary exposure to artificial light.]
Diluent: Methanol and diethylamine (19:1) Standard solution: Dilute 1 volume of the Sample solution with 200 volumes of Diluent (0.1 mg/mL).C19H22N2OS · C4H4O4 442.53
Sample solution: 20.0 mg/mL in DiluentEthanone, 1-[10-[3-(dimethylamino)propyl]-10H-phenothiazin-2- Developing solvent system: n-Heptane, isobutyl alcohol,yl]-, (Z)-2-butenedioate (1:1); and diethylamine (75:17:8)10-[3-(Dimethylamino)propyl]phenothiazin-2-yl methyl ketone
Chromatographic systemmaleate (1:1) [3598-37-6]. (See Chromatography ⟨621⟩, Thin-Layer Chromatography.) Mode: TLCDEFINITION Adsorbent: 0.25-mm layer of chromatographic silica gelAcepromazine Maleate contains NLT 98.0% and NMT 101.0% mixtureof C19H22N2OS · C4H4O4, calculated on the anhydrous basis.
Application volume: 10 µL[NOTE—Throughout the following procedures, protect samples, Analysisthe USP Reference Standard, and solutions containing them, Samples: Standard solution and Sample solutionby conducting the procedures without delay, under subdued Develop the chromatogram in the Developing solventlight, or using low-actinic glassware.] system until the solvent front has moved three-fourths
IDENTIFICATION the length of the plate. Examine the plate under short- • A. INFRARED ABSORPTION ⟨197K⟩ wavelength UV light. • B. The retention time of the peak from the Sample solution Acceptance criteria: No spot, other than the principal
corresponds to that of the Standard solution, as obtained in acepromazine spot and any at the origin, observed in the the Assay. chromatogram of the Sample solution is more intense than
the principal spot observed in the chromatogram of the ASSAY Standard solution (0.5%). • PROCEDURE
Solution A: Add 6 mL of triethylamine to 700 mL of water, SPECIFIC TESTS and adjust with phosphoric acid to a pH of 2.5. • MELTING RANGE OR TEMPERATURE ⟨741⟩: 136°–139°…
Acebutolol Hydrochloride Acetazolamide
Acepromazine Maleate Acetazolamide Oral Suspension
Acepromazine Maleate Injection Acetazolamide Tablets
Acepromazine Maleate Tablets Glacial Acetic Acid
Acetaminophen Acetic Acid Irrigation
Acetaminophen Oral Solution Acetohexamide
Acetaminophen Suppositories Acetohydroxamic Acid
Acetaminophen Tablets Acetylcholine Chloride
Acetaminophen and Aspirin Tablets Acetylcysteine
Acetaminophen, Aspirin, and Caffeine Tablets Acetylcysteine Solution
Acetaminophen and Caffeine Tablets Acetylcysteine and Isoproterenol Hydrochloride Inhalation Solution
Capsules Containing at Least Three of the Following—Acet- aminophen and Salts of Chlorpheniramine, Dex- Acitretin tromethorphan, and Phenylpropanolamine
Acitretin Capsules Oral Solution Containing at Least Three of the Following—
AcyclovirAcetaminophen and Salts of Chlorpheniramine, Dex- tromethorphan, and Phenylpropanolamine Acyclovir Capsules Tablets Containing at Least Three of the Following—Acet- Acyclovir for Injection aminophen and Salts of Chlorpheniramine, Dex- tromethorphan, and Phenylpropanolamine Acyclovir Ointment
Capsules Containing at Least Three of the Following—Acet- Acyclovir Oral Suspension aminophen and Salts of Chlorpheniramine, Dex-
Acyclovir Tabletstromethorphan, and Pseudoephedrine AdenineOral Powder Containing at Least Three of the Following—
Acetaminophen and Salts of Chlorpheniramine, Dex- Adenosine tromethorphan, and Pseudoephedrine
Adenosine Injection Oral Solution Containing at Least Three of the Following— Acetaminophen and Salts of Chlorpheniramine, Dex- Medical Air tromethorphan, and Pseudoephedrine
Alanine Tablets Containing at Least Three of the Following—Acet-
Albendazoleaminophen and Salts of Chlorpheniramine, Dex- tromethorphan, and Pseudoephedrine Albendazole Oral Suspension Acetaminophen, Chlorpheniramine Maleate, and Dex- Albendazole Tablets tromethorphan Hydrobromide Tablets
Albumin Human Acetaminophen and Codeine Phosphate Capsules
Albuterol Acetaminophen and Codeine Phosphate Oral Solution
Albuterol Sulfate Acetaminophen and Codeine Phosphate Oral Suspension
Albuterol Tablets Acetaminophen and Codeine Phosphate Tablets
Alclometasone Dipropionate Acetaminophen, Dextromethorphan Hydrobromide, Doxyl- amine Succinate, and Pseudoephedrine Hydrochloride Oral Alclometasone Dipropionate Cream Solution
Alclometasone Dipropionate Ointment Acetaminophen and Diphenhydramine Citrate Tablets
Alcohol Acetaminophen, Diphenhydramine Hydrochloride, and
Dehydrated AlcoholPseudoephedrine Hydrochloride Tablets
Copyright 2008 The United States Pharmacopeial Convention. All Rights Reserved. For Discussion Purposes Only — Not for Dissemination
2 / MONOGRAPH LIST USP 32
Dehydrated Alcohol Injection Aluminum Chloride
Rubbing Alcohol Aluminum Chlorohydrate
Alendronate Sodium Aluminum Chlorohydrex Polyethylene Glycol
Alendronate Sodium Tablets Aluminum Chlorohydrex Propylene Glycol
Alfentanil Hydrochloride Aluminum Dichlorohydrate
Alfuzosin Hydrochloride Aluminum Dichlorohydrex Polyethylene Glycol
Allantoin Aluminum Dichlorohydrex Propylene Glycol
Allopurinol Aluminum Hydroxide Gel
Aloe Aluminum Phosphate Gel
Alprostadil Aluminum Sesquichlorohydrex Propylene Glycol
Alprostadil Injection Aluminum Subacetate Topical Solution
Alteplase Aluminum Sulfate
Alteplase for Injection Aluminum Sulfate and Calcium Acetate for Topical Solution
Altretamine Aluminum Sulfate and Calcium Acetate Tablets for Topical Solution
Altretamine Capsules Aluminum Zirconium Octachlorohydrate
Ammonium Alum Aluminum Zirconium Octachlorohydrate Solution
Potassium Alum Aluminum Zirconium Octachlorohydrex Gly
Alumina and Magnesia Oral Suspension Aluminum Zirconium Octachlorohydrex Gly Solution
Alumina and Magnesia Tablets Aluminum Zirconium Pentachlorohydrate
Alumina, Magnesia, and Calcium Carbonate Oral Suspension Aluminum Zirconium Pentachlorohydrate Solution
Alumina, Magnesia, and Calcium Carbonate Tablets Aluminum Zirconium Pentachlorohydrex Gly
Alumina, Magnesia, and Calcium Carbonate Chewable Tablets Aluminum Zirconium Pentachlorohydrex Gly Solution
Alumina, Magnesia, Calcium Carbonate, and Simethicone Aluminum Zirconium Tetrachlorohydrate Tablets
Aluminum Zirconium Tetrachlorohydrate Solution Alumina, Magnesia, Calcium Carbonate, and Simethicone
Aluminum Zirconium Tetrachlorohydrex GlyChewable Tablets Aluminum Zirconium Tetrachlorohydrex Gly SolutionAlumina, Magnesia, and Simethicone Oral Suspension Aluminum Zirconium TrichlorohydrateAlumina, Magnesia, and Simethicone Tablets Aluminum Zirconium Trichlorohydrate SolutionAlumina, Magnesia, and Simethicone Chewable Tablets Aluminum Zirconium Trichlorohydrex GlyAlumina and Magnesium Carbonate Oral Suspension Aluminum Zirconium Trichlorohydrex Gly SolutionAlumina and Magnesium Carbonate Tablets Amantadine HydrochlorideAlumina, Magnesium Carbonate, and Magnesium Oxide
Tablets Amantadine Hydrochloride Capsules Alumina and Magnesium Trisilicate Oral Suspension Amantadine Hydrochloride Oral Solution Alumina and Magnesium Trisilicate Tablets Amcinonide Aluminum Acetate Topical Solution
Copyright 2008 The United States Pharmacopeial Convention. All Rights Reserved. For Discussion Purposes Only — Not for Dissemination
USP 32 MONOGRAPH LIST / 3
Amcinonide Cream Amitriptyline Hydrochloride
Amifostine Amitriptyline Hydrochloride Tablets
Amikacin Aromatic Ammonia Spirit
Amikacin Sulfate Ammonium Chloride
Amiloride Hydrochloride and Hydrochlorothiazide Tablets Ferric Ammonium Citrate for Oral Solution
Amiloxate Ammonium Molybdate
Aminobenzoate Potassium for Oral Solution Amobarbital Sodium for Injection
Aminobenzoate Potassium Tablets Amodiaquine
Aminobenzoate Sodium Amodiaquine Hydrochloride
Aminobenzoic Acid Gel Amoxapine
Aminocaproic Acid Amoxicillin
Aminocaproic Acid Oral Solution Amoxicillin Capsules
Aminocaproic Acid Tablets Amoxicillin Intramammary Infusion
Aminoglutethimide Amoxicillin for Injectable Suspension
Aminoglutethimide Tablets Amoxicillin Oral Suspension
Aminohippurate Sodium Injection Amoxicillin for Oral Suspension
Aminohippuric Acid Amoxicillin Tablets
Aminopentamide Sulfate Injection Amoxicillin and Clavulanate Potassium for Oral Suspension
Aminopentamide Sulfate Tablets Amoxicillin and Clavulanate Potassium Tablets
Aminophylline Amphetamine Sulfate
Aminophylline Rectal Solution Amphotericin B Cream
Aminophylline Suppositories Amphotericin B for Injection
Aminophylline Tablets Amphotericin B Lotion
Aminophylline Delayed-Release Tablets Amphotericin B Ointment
Aminosalicylate Sodium Ampicillin
Aminosalicylic Acid Ampicillin Capsules
Amitraz Ampicillin Soluble Powder
Copyright 2008 The United States Pharmacopeial Convention. All Rights Reserved. For Discussion Purposes Only — Not for Dissemination
4 / MONOGRAPH LIST USP 32
Ampicillin for Oral Suspension Arginine Hydrochloride
Ampicillin Tablets Arginine Hydrochloride Injection
Ampicillin and Probenecid for Oral Suspension Arsanilic Acid
Ampicillin Sodium Ascorbic Acid
Amprolium Ascorbic Acid Oral Solution
Amprolium Soluble Powder Ascorbic Acid Tablets
Amprolium Oral Solution Aspartic Acid
Amyl Nitrite Aspirin
Anileridine Aspirin Capsules
Anileridine Hydrochloride Aspirin Suppositories
Anthralin Aspirin Delayed-Release Tablets
Anthralin Ointment Aspirin Extended-Release Tablets
Anthrax Vaccine Adsorbed Aspirin, Alumina, and Magnesia Tablets
Anticoagulant Citrate Dextrose Solution Aspirin, Alumina, and Magnesium Oxide Tablets
Anticoagulant Citrate Phosphate Dextrose Solution Aspirin, Caffeine, and Dihydrocodeine Bitartrate Capsules
Anticoagulant Citrate Phosphate Dextrose Adenine Solution Aspirin and Codeine Phosphate Tablets
Anticoagulant Heparin Solution Aspirin, Codeine Phosphate, Alumina, and Magnesia Tablets
Anticoagulant Sodium Citrate Solution Astemizole
Antihemophilic Factor Astemizole Tablets
Cryoprecipitated Antihemophilic Factor Atenolol
Antimony Sodium Tartrate Atenolol Oral Solution
Antipyrine Atenolol Tablets
Antipyrine, Benzocaine, and Phenylephrine Hydrochloride Atovaquone Otic Solution
Atovaquone Oral Suspension Antithrombin III Human
Atracurium Besylate Antivenin (Crotalidae) Polyvalent
Atracurium Besylate Injection Antivenin (Latrodectus mactans)
Atropine Antivenin (Micrurus fulvius)
Atropine Sulfate Apomorphine Hydrochloride
Atropine Sulfate Ophthalmic Solution Apraclonidine Ophthalmic Solution
Atropine Sulfate Tablets Aprotinin
Activated Attapulgite Aprotinin Injection
Colloidal Activated Attapulgite Arginine
Copyright 2008 The United States Pharmacopeial Convention. All Rights Reserved. For Discussion Purposes Only — Not for Dissemination
USP 32 MONOGRAPH LIST / 5
Aurothioglucose Injectable Suspension Azathioprine Tablets
Avobenzone Azathioprine Sodium for Injection
Azaperone Azithromycin
Azatadine Maleate Tablets Aztreonam
Copyright 2008 The United States Pharmacopeial Convention. All Rights Reserved. For Discussion Purposes Only — Not for Dissemination
(Comment on this Monograph)
132270
AnalysisAcarbose Samples: Standard solution and Sample solutionid=m115=Acarbose=A- Calculate the percentage of C25H43NO18 in the portion ofMonos.pdf) Acarbose taken:
Result = (rU/rS) × (CS/CU) × 100
rU = peak response from the Sample solution rS = peak response from the Standard solution CS = concentration of USP Acarbose RS in the
Standard solution (mg/mL) CU = concentration of the Sample solution (mg/mL)C25H43NO18 645.60
Acceptance criteria: 95.0%–102.0%D-Glucose, O-4,6-dideoxy-4-[[[1S-(1α,4α,5β,6α)]-4,5,6- trihydroxy-3-(hydroxymethyl)-2-cyclohexen-1-yl]amino]-α-D- IMPURITIES glucopyranosyl-(1→4)-O-α-D-glucopyranosyl-(1→4)-; Inorganic Impurities
O-4,6-Dideoxy-4-[[(1S,4R,5S,6S)-4,5,6-trihydroxy-3- • RESIDUE ON IGNITION ⟨281⟩: NMT 0.2%, determined on 1.0 g (hydroxymethyl)-2-cyclohexen-1-yl]amino]-α-D- • HEAVY METALS, Method II ⟨231⟩: NMT 20 ppm glucopyranosyl-(1→4)-O-α-D-glucopyranosyl-(1→4)-D- Organic Impurities glucose [56180-94-0]. • PROCEDURE
Mobile phase, System suitability solution, andDEFINITION Chromatographic system: Proceed as directed in theAcarbose is produced by certain strains of Actinoplanes Assay.utahensis. It contains NLT 95.0% and NMT 102.0% of
Sample stock solution: Use the Sample solution, asC25H43NO18, calculated on the anhydrous basis. directed in the Assay.
Sample solution: Sample stock solution and water (1:99)IDENTIFICATION Analysis• A. INFRARED ABSORPTION ⟨197K⟩ Samples: Sample stock solution and Sample solution• B. The retention time of the Sample solution corresponds to Calculate the percentage of each impurity in the portionthat of the Standard solution, as obtained in the Assay. of Acarbose taken:
ASSAY Result = (ri/ra) × RRF × 100• PROCEDURE
Solution A: 0.6 mg/mL of monobasic potassium phosphate ri = peak response for each impurityand 0.35 mg/mL of dibasic sodium phosphate ra = response of the main acarbose peak in theMobile phase: Acetonitrile and Solution A (3:1)
chromatogram of the Sample solutionSystem suitability solution: Reconstitute a vial of USP RRF = relative response factor for each impurity, asAcarbose System Suitability Mixture RS in 1 mL of water.
listed in the Impurity TableStandard solution: Reconstitute a vial of USP Acarbose RS Acceptance criteriain 5.0 mL of water. Individual impurities: See Impurity Table.Sample solution: 20 mg/mL of Acarbose in water Total impurities: NMT 3.0%Chromatographic system
(See Chromatography ⟨621⟩, System Suitability.) Mode: LC Impurity Table Detector: UV 210 nm
Relative Relative AcceptanceColumn: 4-mm × 25-cm; packing L8 Retention Response Criteria,Temperature: 35°
Name Time Factor NMT (%)Flow rate: 2 mL/min Impurity Aa 0.9 1 0.6Injection size: 10 µL
System suitability Impurity Bb 0.8 1.6 0.5 Sample: System suitability solution
Impurity Cc 1.2 1 1.5[NOTE—Identify the acarbose peak and the peaks due to Impurity Dd 0.5 1.33 1.0the impurities listed in the Impurity Table.]
Suitability requirements Impurity Ee 1.7 0.8 0.2 Height to valley ratio: NLT 1.2 for the impurity A peak,
Impurity Ff 1.9 0.8 0.3and the valley between the impurity A peak and the Impurity Gg 2.2 0.8 0.3acarbose peak
[NOTE—The chromatogram obtained is similar to the Impurity Hh 0.6 1 0.2 chromatogram supplied with USP Acarbose System Suitability Mixture RS.]
Copyright 2008 The United States Pharmacopeial Convention. All Rights Reserved. For Discussion Purposes Only — Not for Dissemination
Impurity Table (continued) USP Acarbose System Suitability Mixture RS
Relative Relative Acceptance Retention Response Criteria,
Name Time Factor NMT (%) Acebutolol Hydrochloride Any individual — — 0.2 id=m125=Acebutolol unknown impurity Hydrochloride=A-Monos.pdf)
aO-4,6-Dideoxy-4-[[(1S,4R,5S,6S)-4,5,6-trihydroxy-3- (hydroxymethyl)cyclohex-2-enyl]amino]-α-D-glucopyranosyl-(1→4)-O-α-D- glucopyranosyl-(1→4)-D-arabino-hex-2-ulopyranose. b(1R,4R,5S,6R)-4,5,6-Trihydroxy-2-(hydroxymethyl)cyclohex-2-enyl 4-O- [4,6-dideoxy-4-[[(1S,4R,5S,6S)-4,5,6-trihydroxy-3- (hydroxymethyl)cyclohex-2-enyl]amino]-α-D-glucopyranosyl]-α-D- glucopyranoside.
Standard solution: 0.14 mg/mL of USP Acebutolol Hydrochloride RS
SPECIFIC TESTS Sample solution: 0.14 mg/mL of Acebutolol Hydrochloride • OPTICAL ROTATION, Specific Rotation ⟨781S⟩: +168° to +183° Chromatographic system
Sample solution: 10 mg/mL (See Chromatography ⟨621⟩, System Suitability.) • PH ⟨791⟩: 5.5–7.5, in a solution containing 50 mg/mL • WATER DETERMINATION, Method Ic ⟨921⟩: NMT 4.0%
ADDITIONAL REQUIREMENTS • PACKAGING AND STORAGE: Preserve in tight containers. • USP REFERENCE STANDARDS ⟨11⟩
USP Acarbose RS
Copyright 2008 The United States Pharmacopeial Convention. All Rights Reserved. For Discussion Purposes Only — Not for Dissemination
USP 32 Official Monographs / Acebutolol 3
Mode: LC ADDITIONAL REQUIREMENTS Detector: UV 254 nm • PACKAGING AND STORAGE: Preserve in tight containers, and Column: 3.9-mm × 30-cm; packing L1 store at controlled room temperature. Flow rate: 2 mL/min • USP REFERENCE STANDARDS ⟨11⟩ Injection size: 10 µL USP Acebutolol Hydrochloride RS
System suitability Sample: Standard solution Suitability requirements Acebutolol Hydrochloride CapsulesColumn efficiency: NLT 1500 theoretical plates Tailing factor: NMT 2.5 id=m127=Acebutolol Relative standard deviation: NMT 2.0% Hydrochloride Capsules=A-Monos.pdf)
Analysis DEFINITIONSamples: Standard solution and Sample solution Acebutolol Hydrochloride Capsules contain the equivalent ofCalculate the percentage of C18H28N2O4 · HCl in the NLT 90.0% and NMT 110.0% of the labeled amount ofAcebutolol Hydrochloride taken: acebutolol (C18H28N2O4).
Result = (rU/rS) × (CS/CU) × 100 IDENTIFICATION • The retention time of the Sample solution corresponds to thatrU = peak response from the Sample solution
of the Standard solution, as obtained in the Assay.rS = peak response from the Standard solution CS = concentration of USP Acebutolol Hydrochloride
ASSAYRS in the Standard solution (mg/mL) • PROCEDURECU = concentration of the Sample solution (mg/mL) Solution A: Dissolve 2.4 g of sodium 1-decanesulfonate inAcceptance criteria: 98.0%–102.0% 1000 mL of water. Adjust with glacial acetic acid to a pH of 3.5.IMPURITIES
Mobile phase: Methanol and Solution A (3:2)Inorganic Impurities Standard solution: 0.22 mg/mL of USP Acebutolol• RESIDUE ON IGNITION ⟨281⟩: NMT 0.1% Hydrochloride RS in methanol• HEAVY METALS, Method II ⟨231⟩: NMT 20 ppm [NOTE—This is equivalent to 0.2 mg/mL of acebutolol.]Organic Impurities
Sample stock solution: Weigh and mix, as completely as• PROCEDURE possible, the contents of NLT 20 Capsules. Transfer a portionStandard solution: 1.0 mg/mL of USP Acebutolol of the powder, equivalent to 200 mg of acebutolol, to aHydrochloride RS in methanol 200-mL volumetric flask. Add 180 mL of methanol, and stirReference solution A: Dilute 3.0 mL of the Standard by mechanical means for 30 min. Dilute with methanol tosolution with methanol to 100 mL. volume.Reference solution B: Dilute 5.0 mL of the Standard
Sample solution: Dilute 5.0 mL of the Sample stock solutionsolution with methanol to 100 mL. with methanol to 25 mL.Sample solution A: 10 mg/mL of Acebutolol
Chromatographic systemHydrochloride in methanol (See Chromatography ⟨621⟩, System Suitability.)Sample solution B: Sample solution A and methanol (1:9) Mode: LCDeveloping solvent system: Butyl alcohol, glacial acetic Detector: UV 254 nmacid, and water (4:1:5) Column: 3.9-mm × 15-cm; 5-µm packing L1Chromatographic system Flow rate: 1 mL/min(See Chromatography ⟨621⟩, Thin-Layer Chromatography.) Injection size: 20 µLMode: TLC
System suitabilityAdsorbent: 0.25-mm layer of chromatographic silica gel Sample: Standard solutionmixture Suitability requirementsApplication volume: 20 µL Tailing factor: NMT 1.5Analysis Relative standard deviation: NMT 2.0%Samples: Standard solution, Reference solution A, Reference
Analysissolution B, Sample solution A, and Sample solution B Samples: Standard solution and Sample solutionProceed as directed in the chapter. Develop the Calculate the percentage of C18H28N2O4 in the Capsuleschromatogram in the Developing solvent system until the taken:solvent front has moved three-fourths the length of the
plate. Examine the plate under short-wavelength UV Result = (rU/rS) × (CS/CU) × (Mr1/Mr2) × 100light.
Acceptance criteria: The chromatograms from Sample rU = peak response from the Sample solutionsolution B and the Standard solution show principal spots at rS = peak response from the Standard solutionthe same RF value. No secondary spot from Sample solution CS = concentration of USP Acebutolol HydrochlorideA, excluding the area at the point of application, is more
RS in the Standard solution (mg/mL)intense than the principal spot of Reference solution A CU = nominal concentration of the Sample solution(0.3%); NMT two secondary spots from Sample solution A
(mg/mL)are more intense than the principal spot of Reference Mr1 = molecular weight of acebutolol, 336.44solution B (0.1%); and the total of all impurities detected in Mr2 = molecular weight of acebutolol hydrochloride,the chromatogram of Sample solution A is NMT 0.5%.
372.89 SPECIFIC TESTS • MELTING RANGE OR TEMPERATURE ⟨741⟩: 140°–144° • PH ⟨791⟩: 4.5–7.0, in a solution (1 in 100) • LOSS ON DRYING ⟨731⟩: Dry it at 105° for 3 h: it loses NMT
1.0% of its weight
Copyright 2008 The United States Pharmacopeial Convention. All Rights Reserved. For Discussion Purposes Only — Not for Dissemination
4 Acebutolol / Official Monographs USP 32
Acceptance criteria: 90.0%–110.0% rS = peak response from the Standard solution CS = concentration of USP Acebutolol Hydrochloride
PERFORMANCE TESTS RS in the Standard solution (µg/mL) • DISSOLUTION ⟨711⟩ CU = nominal concentration of the Sample solution
Medium: Water; 900 mL (µg/mL) Apparatus 2: 50 rpm Mr1 = molecular weight of acebutolol, 336.44 Time: 30 min Mr2 = molecular weight of acebutolol hydrochloride, Sample solution: Sample per Dissolution ⟨711⟩. 372.89 Standard solution: USP Acebutolol Hydrochloride RS in Test 2 Medium Solution A: Prepare as directed in the Assay.
Spectrometric conditions Mobile phase: Methanol and Solution A (1:1) Mode: UV Standard solution: Transfer 30 mg of USP Acebutolol Analytical wavelength: 232 nm Hydrochloride RS to a 50-mL volumetric flask. Add 12 mL Analysis: Determine the amount of C18H28N2O4 dissolved of methanol, swirl to dissolve, and dilute with Mobile by employing the UV absorption on filtered portions of the phase to volume. Dilute a volume of this stock solution Sample solution in comparison with a Standard solution in with Mobile phase to obtain a concentration of 1.4 µg/mL the same Medium. of USP Acebutolol Hydrochloride RS.
Tolerances: NLT 80% (Q) of the labeled amount of Sample solution: Transfer a portion of the contents of 20 C18H28N2O4 is dissolved. opened Capsules, equivalent to 250 mg of acebutolol, to
• UNIFORMITY OF DOSAGE UNITS ⟨905⟩: Meet the requirements a 100-mL volumetric flask, add 25 mL of methanol, and shake by mechanical means for 15 min. Dilute with MobileIMPURITIES phase to volume. Centrifuge a portion of this solution,Organic Impurities and transfer 10.0 mL of the clear supernatant to a 100-mL• PROCEDURE volumetric flask. Dilute with Mobile phase to volume.Test 1 Chromatographic systemSolution A: Prepare as directed in the Assay. (See Chromatography ⟨621⟩, System Suitability.)Mobile phase: Methanol and Solution A (44:56) Mode: LCDiluent: Methanol and Solution A (1:1) Detector: UV 240 nmStandard solution: Transfer 30 mg of USP Acebutolol Column: 3.9 mm × 15 cm; 4-µm packing L1Hydrochloride RS to a 50-mL volumetric flask. Add 12 mL Flow rate: 1 mL/minof methanol, swirl to dissolve, and dilute with Diluent to Injection size: 70 µLvolume. Dilute a volume of this solution with Diluent to System suitabilityobtain a concentration of 1.4 µg/mL of USP Acebutolol Sample: Standard solutionHydrochloride RS. Suitability requirementsSample solution: Transfer a portion of the contents of 20 Relative standard deviation: NMT 6.0%opened Capsules, equivalent to 250 mg of acebutolol, to Analysisa 100-mL volumetric flask, add 25 mL of methanol, and Samples: Mobile phase, Standard solution, and Sampleshake by mechanical means for 15 min. Dilute with solutionDiluent to volume. Centrifuge a portion of this solution, Calculate the percentage of each impurity eluting afterand transfer 10.0 mL of the clear supernatant to a 100-mL the acebutolol peak in the portion of Capsules taken:volumetric flask. Dilute with Diluent to volume.
Chromatographic system Result = (rU/rS) × (CS/CU) × (Mr1/Mr2) × 100 (See Chromatography ⟨621⟩, System Suitability.) Mode: LC rU = peak response for any individual impurity from Detector: UV 240 nm the Sample solution Column: 3.9-mm ×15-cm; 4-µm packing L1 rS = peak response from the Standard solution Flow rate: 1 mL/min CS = concentration of USP Acebutolol Hydrochloride Injection size: 35 µL RS in the Standard solution (µg/mL)
System suitability CU = nominal concentration of the Sample solution Sample: Standard solution (µg/mL) Suitability requirements Mr1 = molecular weight of acebutolol, 336.44 Relative standard deviation: NMT 6.0% Mr2 = molecular weight of acebutolol hydrochloride,
Analysis 372.89 Samples: Diluent, Standard solution, and Sample solution Acceptance criteria
[NOTE—Record the chromatograms for two times the Test 1: NMT 0.5% of any individual impurity retention time of acebutolol, and measure the Test 2: NMT 0.5% of any individual impurity responses for all the peaks, disregarding any peaks Sum of impurities found in Test 1 and Test 2: NMT corresponding to those obtained from the Diluent.] 1.0%
Calculate the percentage of each impurity eluting prior to the acebutolol peak in the portion of Capsules taken: ADDITIONAL REQUIREMENTS
• PACKAGING AND STORAGE: Preserve in tight containers, and Result = (rU/rS) × (CS/CU) × (Mr1/Mr2) × 100 store at controlled room temperature.
• USP REFERENCE STANDARDS ⟨11⟩ rU = peak response for any individual impurity from USP Acebutolol Hydrochloride RS
the Sample solution
Copyright 2008 The United States Pharmacopeial Convention. All Rights Reserved. For Discussion Purposes Only — Not for Dissemination
(Comment on this Monograph)
(Comment on this Monograph)
Acceptance criteria: 98.0%–101.0%Acepromazine Maleate id=m134=Acepromazine IMPURITIES
Maleate=A-Monos.pdf) Inorganic Impurities • RESIDUE ON IGNITION ⟨281⟩: NMT 0.2% Organic Impurities • PROCEDURE
[NOTE—Conduct this test without exposure to daylight, and with the minimum necessary exposure to artificial light.]
Diluent: Methanol and diethylamine (19:1) Standard solution: Dilute 1 volume of the Sample solution with 200 volumes of Diluent (0.1 mg/mL).C19H22N2OS · C4H4O4 442.53
Sample solution: 20.0 mg/mL in DiluentEthanone, 1-[10-[3-(dimethylamino)propyl]-10H-phenothiazin-2- Developing solvent system: n-Heptane, isobutyl alcohol,yl]-, (Z)-2-butenedioate (1:1); and diethylamine (75:17:8)10-[3-(Dimethylamino)propyl]phenothiazin-2-yl methyl ketone
Chromatographic systemmaleate (1:1) [3598-37-6]. (See Chromatography ⟨621⟩, Thin-Layer Chromatography.) Mode: TLCDEFINITION Adsorbent: 0.25-mm layer of chromatographic silica gelAcepromazine Maleate contains NLT 98.0% and NMT 101.0% mixtureof C19H22N2OS · C4H4O4, calculated on the anhydrous basis.
Application volume: 10 µL[NOTE—Throughout the following procedures, protect samples, Analysisthe USP Reference Standard, and solutions containing them, Samples: Standard solution and Sample solutionby conducting the procedures without delay, under subdued Develop the chromatogram in the Developing solventlight, or using low-actinic glassware.] system until the solvent front has moved three-fourths
IDENTIFICATION the length of the plate. Examine the plate under short- • A. INFRARED ABSORPTION ⟨197K⟩ wavelength UV light. • B. The retention time of the peak from the Sample solution Acceptance criteria: No spot, other than the principal
corresponds to that of the Standard solution, as obtained in acepromazine spot and any at the origin, observed in the the Assay. chromatogram of the Sample solution is more intense than
the principal spot observed in the chromatogram of the ASSAY Standard solution (0.5%). • PROCEDURE
Solution A: Add 6 mL of triethylamine to 700 mL of water, SPECIFIC TESTS and adjust with phosphoric acid to a pH of 2.5. • MELTING RANGE OR TEMPERATURE ⟨741⟩: 136°–139°…