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Certificate of Analysis: 4-Aminophenol

This document provides a certificate of analysis for a certified reference material of 4-aminophenol (paracetamol impurity K). It summarizes that the certified purity is 97.8% with an uncertainty of 0.4% according to tests including HPLC assays and mass balance calculations. The reference material has been tested for identity, purity, residual solvents, water content, and homogeneity.

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Laurențiu Mihai Bălan
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697 views6 pages

Certificate of Analysis: 4-Aminophenol

This document provides a certificate of analysis for a certified reference material of 4-aminophenol (paracetamol impurity K). It summarizes that the certified purity is 97.8% with an uncertainty of 0.4% according to tests including HPLC assays and mass balance calculations. The reference material has been tested for identity, purity, residual solvents, water content, and homogeneity.

Uploaded by

Laurențiu Mihai Bălan
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Download as PDF, TXT or read online on Scribd
You are on page 1/ 6

Certificate of Analysis

ISO GUIDE 34
ANAB Cert# AR-1470 4-AMINOPHENOL
(Acetaminophen Related Compound K)
ISO/IEC 17025
ANAB Cert# AT-1467 (Paracetamol Impurity K)
CERTIFIED REFERENCE MATERIAL

CERTIFIED PURITY: 97.8%, Ucrm = 0.4% k = 2


(Mass Balance/as is basis)

NOMINAL PACKAGE SIZE: 1g

CATALOG #: PHR1148 LOT #: LRAA7699

CERTIFICATE VERSION: LRAA7699.2 ISSUE DATE: 11 August 2016


Note: Certificates may be updated due to Pharmacopeial Lot changes or the availability of new data.
Check our website at: www.sigma-aldrich.com for the most current version.

CRM EXPIRATION: 31 December 2019 (Proper Storage and Handling Required).

RECEIPT DATE: ________________


Note: this space is provided for convenience only and its use is not required.

STORAGE: Store at Room Temperature, keep container tightly closed. Attachment of a


20 mm aluminum crimp seal recommended for unused portions.

CHEMICAL FORMULA: C6H7NO MW: 109.13

PHYSICAL DESCRIPTION: White to beige powder in amber vial CAS #: 123-30-8

HAZARDS: Read Safety Data Sheet before using. All chemical reference materials
should be considered potentially hazardous and should be used only by qualified
laboratory personnel.

Page 1 of 6
INSTRUCTIONS FOR USE: Do not dry, use as is. The internal pressure of the container
may be slightly different from the atmospheric pressure at the user’s location. Open
slowly and carefully to avoid dispersion of the material. This material is intended for
R&D use only. Not for drug, household or other uses.

TRACEABILITY ASSAY
Comparative assay demonstrates direct traceability to Pharmacopeial Standards

METHOD: HPLC (ref.: Adapted from Acetaminophen, USP37)


Column: Ascentis Express C8, 4.6 x 100mm, 2.7µm
Mobile Phase A: 1.7g/L KH2PO4 + 1.8g/L Na2HPO4 in Water
Mobile Phase B: Methanol
Gradient:
Time (min) %A %B
0-3 99 1
3-7 99-19 1-81
7-7.5 19-99 81-1
Flow Rate: 0.8mL/min
Column Temperature: 35ºC
Injection: 2µL
Detector: 230nm

ASSAY vs. USP REFERENCE STANDARD (as is basis)


ASSAY VALUE vs. USP LOT
99.0% R009S0
Labeled Content = 0.99mg/mg

Representative Chromatogram from Lot: LRAA7699 Analysis

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PURITY DETERMINATION BY MASS BALANCE

CHROMATOGRAPHIC IMPURITY ANALYSIS


METHOD: HPLC (ref.: Adapted from Acetaminophen, USP37)

See Assay

Impurities Detected:
Impurity 1: 0.7% Impurity 2: 0.1%
Impurity 3: 0.7%

Total Impurities: 1.6%

Representative Chromatogram from Lot: LRAA7699 Impurity Analysis

RESIDUAL SOLVENTS
Method: GC-MS Headspace (ref.: Residual Solvents <467>, USP34)
Column: DB-1301
Carrier gas: He
Flow: 1.2mL/min
Split Ratio: 1:5
Injection/Temperature: 1µl/250°C
Temperature Program: 40°C for 20min, 10°C/min to 240°C, hold 20min

Solvents Detected: None

WATER DETERMINATION
Method: Karl Fisher titration
Mean of three measurements, Water Content = 0.01%

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RESIDUE ANALYSIS
Method: Sulfated Ash
Sample Size: ~100mg
Mean of three measurements, Residue = 0.6%

CERTIFIED PURITY BY MASS BALANCE [100% - Impurities (normalized)]

97.8% Ucrm = ±0.4%, k = 2


(as is basis)

IDENTIFICATION TESTS
INFRARED SPECTROPHOTOMETRY (Comparative identification analysis
demonstrates direct traceability to Pharmacopeial standards)

Page 4 of 6
1
H NMR (Data provided by an external laboratory; not in scope of accreditation)

Consistent with structure

HOMOGENEITY ASSESSMENT
Homogeneity was assessed in accordance with ISO Guide 35. Completed units were
sampled using a random stratified sampling protocol. The results of chemical analysis
were then compared by Single Factor Analysis of Variance (ANOVA). The uncertainty
due to homogeneity was derived from the ANOVA. Heterogeneity was not detected
under the conditions of the ANOVA.

Analytical Method: HPLC Sample size: ~10mg

UNCERTAINTY STATEMENT
Uncertainty values in this document are expressed as Expanded Uncertainty (Ucrm)
corresponding to the 95% confidence interval. Ucrm is derived from the combined
standard uncertainty multiplied by the coverage factor k, which is obtained from a t-
distribution and degrees of freedom. The components of combined standard uncertainty
include the uncertainties due to characterization, homogeneity, long term stability, and
short term stability (transport). The components due to stability are generally considered
to be negligible unless otherwise indicated by stability studies.

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STABILITY ASSESSMENT
Significance of the stability assessment will be demonstrated if the analytical result of the
study and the range of values represented by the Expanded Uncertainty do not overlap the
result of the original assay and the range of its values represented by the Expanded
Uncertainty. The method employed will usually be the same method used to characterize
the assay value in the initial evaluation.
Long Term Stability Evaluation - An assessment, or re-test, versus a Compendial
Reference Standard may be scheduled, within the 3 year anniversary date of a release of a
Secondary Standard. The re-test interval will be determined on a case-by-case basis.
Short Term Stability Study - It is useful to assess stability under reasonably anticipated,
short term transport conditions by simulating exposure of the product to humidity and
temperature stress. This type of study is conducted under controlled conditions of
elevated temperature and humidity.

__________________________________ _______________________________
Operations Manager QA Supervisor

APPENDIX

Original Release Date: 01 May 2015

Manufactured and certified by Sigma-Aldrich RTC, Inc.


2931 Soldier Springs Rd, Laramie WY, USA 82070 Page 6 of 6
(Phone): 1-307-742-5452 (Fax): 1-855-831-9212
email: RTCTechGroup@sial.com

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