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M7(R2) ADDENDUM: APPLICATION OF THE PRINCIPLES OF THE ICH M7 GUIDELINE TO CALCULATION OF COMPOUND-SPECIFIC ACCEPTABLE INTAKES: Guidance for Industry

FinalCenter for Drug Evaluation and Research Center for Biologics Evaluation and Research07/25/2023
Quality StandardsOxidative stressMode of ActionData IntegrityThreshold of Toxicological ConcernHuman Risk Assessment

Description

The Food and Drug Administration (FDA or Agency) is announcing the availability of a final guidance for industry entitled “M7(R2) Assessment and Control of DNA Reactive (Mutagenic) Impurities in Pharmaceuticals to Limit Potential Carcinogenic Risk” (M7(R2) Guidance) and two supplemental documents entitled “M7(R2) Addendum: Application of the Principles of the ICH M7 Guidance to Calculation of Compound-Specific Acceptable Intakes” (M7(R2) Addendum) and “M7(R2) Assessment and Control of DNA Reactive (Mutagenic) Impurities in Pharmaceuticals to Limit Potential Carcinogenic Risk Questions and Answers” (M7(R2) Questions and Answers). The M7(R2) Guidance, M7(R2) Addendum, and M7(R2) Questions and Answers were prepared under the auspices of the International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use (ICH). The guidance and supplemental documents are intended to harmonize the considerations for assessment and control of DNA reactive (mutagenic) impurities.

Key Topics

Terms and concepts identified from this document

Scope & Applicability

Product Classes

4
Pharmaceuticals

Scope of the mutagenic impurities assessment; AI calculated for potential pharmaceutical impurities; General context of ICH guidelines for industry; benzyl chloride as an impurity in drugs; Hydrazine is used in the synthesis of these products; Derivation of an AI for inhaled pharmaceuticals; Application of limits in pharmaceutical products; Application of ICH M7 principles to pharmaceutical impurities.

Drug product

formaldehyde as a drug product impurity

Active Pharmaceutical Ingredient

limit in active pharmaceutical ingredient (API) or drug product

Pharmaceutical Impurity

Low, nontoxic concentrations of substances in drugs

Stakeholders

2
Heavy drinkers

elevated risk of head and neck cancers associated with acetaldehyde exposure in heavy drinkers

Manufacturer

Entity responsible for submitting NDINs

Regulatory Context

Regulatory Activities

3
Marketing application submissions

ICH guidelines standardized safety reporting and marketing application submissions

Acceptable Intake calculation

regulatory process of deriving safety limits from carcinogenicity data

Compound-specific risk assessments

Applied to derive AIs instead of TTC-based values

Document Types

4
NTP Technical Report

Selected to calculate the AI for acrylonitrile; Source of toxicology and carcinogenesis studies

Carcinogen Potency Database

Source for TD50 values

Carcinogenic Potency Database

source for TD50 values and carcinogenicity data

Chronic Bioassay

Lijinsky study of benzyl chloride

Attributes

10
Maximum tolerated dose

Dose selection criterion for carcinogenicity studies; criteria for adequacy of the rat study; Virtually Safe Dose Based on the Maximum Tolerated Dose.; Based on the Maximum Tolerated Dose for Rodent Bioassays.

Virtually Safe Dose

Quick Estimate of the Regulatory Virtually Safe Dose.

Tidal volume

500 milliliters (mL) for adult males and 400 mL for adult females

Dose Response

The positive dose response was not statistically significant.

NOAEL

No-observed adverse effect level for histological changes

Group 2B

Classification as possibly carcinogenic to humans

Tolerable Daily Intake

WHO defined a TDI for styrene of 7.7 µg/kg/day.

Category D

EPA classification for not classifiable as to human carcinogenicity

Group 3

IARC classification for inadequate evidence of carcinogenicity

Group 2A

IARC classification for glycidol as probably carcinogenic

Technical Details

Substances

10
Acetaldehyde

CAS# 75-07-0; Formed endogenously in the human body from metabolism of ethanol; Acetaldehyde is a strong electrophile and is capable of reacting with strong nucleophiles; Pathobiological Effects of Acetaldehyde in Cultured Human Epithelial Cells; Metabolite of vinyl acetate responsible for genotoxicity; oral PDE recommended is based on that derived for acetaldehyde

Albuterol sulfate

actuator with formaldehyde as an impurity

para-Chloronitrobenzene

Carcinogenicity and Chronic Toxicity of para-Chloronitrobenzene in Rats and Mice.

Acetic acid

Breakdown product of vinyl acetate

Styrene-7,8-oxide

Main metabolite of styrene, clearly mutagenic; Styrene-7,8-oxide is a metabolite of styrene classified as probably carcinogenic.

CYP2E1

Isozyme responsible for methyl chloride metabolism in mouse kidney

Hydroxyl radicals

Reactive species generated from hydrogen peroxide in the presence of metals

Catalase

Enzyme that reduces hydrogen peroxide to water and oxygen

Hydrazine sulfate

administered to mice for 25 weeks in a multidose gavage study

Hydrazine sulphate

used in the treatment of tuberculosis and sickle cell anemia

Testing Methods

10
Bacterial reverse mutation assay

Ames test used as main criterion for determining mutagenicity; Ames test used to evaluate DMS mutagenicity; Ames test used for mutagenicity testing

Chronic Inhalation Toxicology Study

Study in Rats and Mice Exposed to Methyl Chloride.

Linear Regression

Plotting the results and using the slope to represent beta results in the following graphs.

Rodent Bioassays

Quick Estimate of the Regulatory Virtually Safe Dose Based on the Maximum Tolerated Dose for Rodent Bioassays.

Genotoxicity data

IARC concluded there is strong evidence that styrene is genotoxic.

HPRT assay

In vitro mammalian gene mutation study

Carcinogenicity studies

Evaluation of hydrogen peroxide safety

Linearized multistage extrapolation

Limit is a linearized multistage extrapolation based on hepatomas

2-year bioassay

standard long-term carcinogenicity study

Mouse micronucleus assay

In vivo test for glycidol

Processes

9
Pharmaceutical manufacturing

Context where mutagenic chemicals are common

Synthesis of pharmaceuticals

Industrial use of vinyl acetate

Oral gavage

method of administration in carcinogenicity bioassays; Method of administration in hamster studies; Studies conducted via oral gavage to assess carcinogenic potency.

Biosynthesis

Formaldehyde essential for amino acid production

Intraperitoneal injection

route used in Van Duuren study for DMCC

Inhalation

route of exposure in carcinogenicity studies; route of exposure for DMCC and DMS; exposure route for hydrazine carcinogenicity studies; Separate AI for inhalation exposure was appropriate; Route of administration in 2-year bioassay; Styrene is reported to be carcinogenic in mice via the inhalation route.

Gavage

Method of oral administration in carcinogenicity studies; oral administration method in Lijinsky study; method of administration in NTP studies for p-chloroaniline; administration in the feed to rats and mice or by gavage; Route of administration in short-term carcinogenicity models; oral route of administration for carcinogenicity studies; Oral gavage study of Wester et al.; Method of administration in carcinogenicity study; Method of administration in NTP studies; Hydrazine sulfate was adminis

Oral carcinogenicity study

An oral carcinogenicity study was conducted in Sprague Dawley rats

Inhalation carcinogenicity study

In rodents, only inhalation carcinogenicity studies are available

Clinical Concepts

10
Tumors

Human relevance of tumors

Carcinoma

Hydrazine calculations were based on female rats

Hepatocellular adenoma

Hydrazine calculations were based on the most sensitive tumor type

Tumor

P is the proportion of animals with the specified tumor type observed at a certain dose.

Pheochromocytoma

calculations were based on the most sensitive tumor type: female rat pheochromocytoma

Nasal tumors

Observed in Sprague-Dawley rats following inhalation

Squamous cell tumors

Styrene-7,8-oxide increased squamous cell tumors in the forestomach.

Alveolar and bronchiolar adenomas

Oral exposure to styrene increased incidence of these tumors in mice.

Renal adenocarcinomas

Observed in male mice at high exposure levels

Duodenal tumors

Statistically significant increases in tumors of the duodenum observed in mice; Tumors observed in mouse drinking water studies

Identified Hazards

Hazards

9
Tumor Induction

The primary safety concern addressed by AI and PDE calculations

Mutagenicity

Hydrogen peroxide is mutagenic and genotoxic in vitro

Explosion risk

Limited the exposure concentration in NTP studies

Carcinogenic

Epichlorohydrin is probably carcinogenic to humans

Genotoxic Hazards

Increases in micronucleated cells that do not indicate hazards

Carcinogenicity

risk assessment for pharmaceuticals affecting the immune system

Genotoxicity

nonlinear dose response associated with the genotoxicity and carcinogenicity of acetaldehyde; Historical perception of aniline; Potential for a mutagenic mode of action

Cytotoxicity

nasal tumors in inhalation carcinogenicity studies were only found at inhalation doses also associated with cytotoxicity

Tumors

Endpoint used to calculate TD50

Standards & References

External Standards

4
OECD 453

OECD 453 Guideline for the Testing of Chemicals: Combined Chronic Toxicity/Carcinogenicity Studies

CPDB

TD50 reported in Carcinogenic Potency Database

OECD guideline 453

Standard followed for carcinogenicity study

OECD

Guidelines for genotoxicity assays

Specifications

6
Acceptable Intakes

Derived for mutagenic impurities with positive carcinogenicity data

215 ppb

concentration limit of formaldehyde in air

Specific migration limit

A limit of 60 ppm styrene into foods is permissible in the EU.

Quality limit of 0.5 percent

Upper limit for acceptable intakes

Permissible Daily Exposures

Calculated using uncertainty factors for threshold-based compounds

Threshold of Toxicological Concern

Default basis for acceptable intakes when specific data is lacking

ICH References (5)

ICH M7

Application of the Principles of the ICH M7 Guidance to Calculation of Compound-Specific Acceptable Intakes; Application of the principles of the ICH M7 guideline to calculation of compound-specific acceptable intakes; principles applied to calculation of compound-specific AIs; application of principles to calculation of compound-specific acceptable intakes; Application of the principles of the ICH M7 guideline to calculation of compound-specific acceptable intakes.

ICH M7(R2)

Assessment and Control of DNA Reactive (Mutagenic) Impurities in Pharmaceuticals to Limit Potential Carcinogenic Risk; Application of the principles of the ICH M7 guideline to calculation of compound-specific acceptable intakes; ICH guidance for industry M7(R2) Assessment and Control of DNA Reactive (Mutagenic) Impurities; Document title and version; Document title and addendum reference; Guidance for assessment and control of DNA reactive impurities.; Assessment and Control of DNA Reactive Impu

ICH Q3C(R8)

Impurities: Guidance for Residual Solvents; Guidance for Industry Q3C(R8) Impurities: Guidance for Residual Solvents used to calculate PDE; ICH guidance for industry Q3C(R8) Impurities: Guidance for Residual Solvents; Used to define the process for deriving the PDE for aniline.; Guidance for Residual Solvents used for breathing volume assumptions; Used for human breathing volume assumptions (28,800 liters/day).; Guidance for Residual Solvents used for calculations

ICH Q3D(R2)

Elemental Impurities; PDE methodology is further explained in ICH Q3D(R2)

ICH S1C(R2)

Dose Selection for Carcinogenicity Studies of Pharmaceuticals

Related CFR Sections (1)

See Also (8)

M7(R2) ADDENDUM: APPLICATION OF THE PRINCIPLES OF THE ICH M7 GUIDELINE TO CALCULATION OF COMPOUND-SPECIFIC ACCEPTABLE INTAKES: Guidance for Industry | Guideline Explorer | BioRegHub