Data Sharing Initiatives Dr Andy Teasdale

Similar documents
ICH Q3D: Practical implementation and the role of excipient data in a risk based approach. Dr Andrew Teasdale

Key Analytical Issues: Sample Preparation, Interferences and Variability. Tim Shelbourn, Eli Lilly and Company

RISK ASSESSMENT, IMPLEMENTATION AND VALIDATION OF ELEMENTAL IMPURITIES FOR ICH Q3D, USP <232><233> AND EP 5.20

Opportunities for Regulatory Relief via In Vitro Dissolution. James E. Polli June 10, 2015

Elemental Impurity Analysis: Technical Challenges and Overview of an Inter-laboratory Study PQRI Elemental Impurities Workshop March 31, 2015

Concept of Elemental Impurities (EI) assessment in finished dosage forms by total extraction testing

PQRI Technical Analytical Challenges Round 2 Interlaboratory Study: Progress and Early Findings

Recovery of non-steroidal anti-inflammatory. drugs from wastes using ionic liquid-based. three-phase partitioning systems

Formulation of Low Dose Medicines - Theory and Practice

Elemental Scientific. Stability. Elemental Scientific

Validating performance of an Agilent 7800 ICP MS for USP <232>/<233> & ICH Q3D/Q2(R1): Elemental Impurity Analysis in Pharmaceuticals

Swiss Medic Training Sampling

THERAPEUTIC GOODS SAMPLING Application to Tablet Manufacture and Ingredients. David Edmonds CMC Regulatory

Research Article. Identification and characterization of unknown impurity in zolmitriptan tablets by a sensitive HPLC method

Using cold vapor generation atomic absorption to determine mercury impurities in pharmaceutical products

Verification of Pharmaceutical Raw Materials Using the Spectrum Two N FT-NIR Spectrometer

EP A1 (19) (11) EP A1 (12) EUROPEAN PATENT APPLICATION. (43) Date of publication: Bulletin 2011/28

Elemental Scientific. Spike Recovery. Elemental Scientific

á233ñ ELEMENTAL IMPURITIES PROCEDURES

Entry Guide for "DIC RAW MATERIAL SURVEY" for Form Version 4.1

Process Raman. Utilisation of Raman spectroscopy for primary and secondary pharmaceutical development. Allyson McIntyre Pharmaceutical Development

Cleaning Memo for January 2017 A Critique of the APIC Guideline

Strategies to minimize the impact of presence of residual solvents in APIs

Methyl Salicylate Technical Package

WO 2014/ Al. 11 December 2014 ( ) P O P C T

Quality by Design in the Development of Analytical Procedures

CHAPTER 7 SUMMARY AND CONCLUSIONS. constitutes the objective of many a research project in the field of pharmaceutical

Preparation of Food and Feed Samples for Metals Analysis

Elemental Scientific. Spike Recovery. Elemental Scientific

Workshop IV Understanding Drug-Excipient Interactions

Properties criteria - BETA

Introduction to E&Ls 1

Stability of pharmaceutical preparations

EP A1 (19) (11) EP A1 (12) EUROPEAN PATENT APPLICATION. (43) Date of publication: Bulletin 2012/42

DEVELOPMENT AND VALIDATION OF SPECTROPHOTOMETRIC METHOD FOR CLOPIDOGREL BISULFATE IN BULK AND FORMULATIONS

Part ONE. Answer ALL questions. For each questions, there is ONE correct answer. Use the multiple choice reader card provided for ALL your answers.

Pharmaceutical Polymers for Tablets and Capsules

Development and Validation of Spectrophotometric Method for Clopidogrel bisulfate in pure and in film coated tablet dosage form

PQRI PODP Extractables & Leachables Workshop

Effect of Alkaline Excipients on The Release Profile of Gliclazide Extended Release Tablets

Welcome to Honors Chemistry!

Mouth Disintegrating Tablets of Taste-Masked Ondansetron HCl

Examples of Method Validation Studies Conducted in Different Economies

Properties criteria - BETA

Multi-Element Analysis of Cannabis using the Agilent 7800 ICP-MS

Multi Analyte Custom Grade Solution. Calcium, Iron, Potassium,

ASAP concept and case studies

10.3 Types of Chemical Reactions

Christin T. Choma TA Instruments, 109 Lukens Drive, New Castle, DE 19720, USA

Global Mineral Sand Industry: Trends and Opportunities ( ) February 2014

Relative Response Factor for Lamivudine and Zidovudine Related substances by RP-HPLC with DAD detection

Indian Journal of Research in Pharmacy and Biotechnology

ICP/MS Multi-Element Standards

Validation of UV Spectrophotometric Method for Determination of Riluzole in Pharmaceutical Dosage Form

Aqueous Enteric Coating Application on Non-Banded Hard Gelatin Capsules

ACZ Laboratories, Inc Downhill Drive Steamboat Springs, CO (800)

Supporting Information Appendix. Arsenic pollution of groundwater in Vietnam exacerbated by deep aquifer exploitation for more than a century

FORMULATION, DEVELOPMENT AND CHARACTERIZATION OF ORAL DISINTEGRAING TABLET OF CIMITIDINE HCL

Determination of Elemental Impurities Ciprofloxacin hydrochloride and Fluconazole via ICP-OES

Particle Size Analysis in the Pharmaceutical Industry

Proposed new USP general chapters <232> and <233> for elemental impurities: The application of ICP-MS for pharmaceutical analysis

Apparent Melting: A New Approach to Detecting Drug-Excipient Incompatibility

Introducing the Morphologi G3 ID The future of particle characterization

Research Paper. (1+cos θ)= +

Determining Elemental Impurities in Pharmaceutical Materials: How to Choose the Right Technique

why open access publication of stability date is essential Mark Santillo Regional QA Officer SW England

Starting Materials For Active Substances

The Chemical Reactions

Green Thick Film Chip Resistors

GOLDPLAY ANNOUNCES FURTHER SAMPLING RESULTS FROM SAN MARCIAL HISTORICAL CORE; CONFIRMS OPEN PIT TARGET NEAR SURFACE WITH gpt AgEq.

Lab: Types of Chemical Reactions Safety is very important when combining chemicals

HPLC-ELSD DETERMINATION OF SODIUM LAURYL SULPHATE AND POLYSORBATE IN NEBIVOLOL DRUG PRODUCT AND DIFFERENT FORMULATION PRODUCTS

The Myanmar Mineral Exploration Handbook

Welcome to Honors Chemistry!

International Journal of PharmTech Research CODEN (USA): IJPRIF, ISSN: , ISSN(Online): Vol.9, No.7, pp , 2016

The comparative verification of calibration curve and background fundamental parameter methods for impurity analysis in drug materials

Rosemary extract liquid

The Use of the ACQUITY QDa Detector for a Selective, Sensitive, and Robust Quantitative Method for a Potential Genotoxic Impurity

GC METHOD FOR QUANTITATIVE DETERMINATION OF RESIDUAL 2-(2-CHLOROETHOXY)ETHANOL (CEE) AND N-METHYL-2-PYRROLIDINONE (NMP) IN QUETIAPINE

Exergetic sustainability assessment of batch versus continuous manufacturing Lessons learned in primary and secondary pharmaceutical manufacturing

Results of the 18 th and 19 th Needle/Leaf Interlaboratory Comparison Tests

RESEARCH AND DEVELOPMENT EFFORT IN DEVELOPING THE OPTIMAL FORMULATIONS FOR NEW TABLET DRUGS

OPTIMIZATION OF FUROSEMIDE LIQUISOLID TABLETS PREPARATION PROCESS LEADING TO THEIR MASS AND SIZE REDUCTION

Chromazurol S Method Method to 0.50 mg/l Al TNTplus 848

Materials for Pharmaceutical Manufacturing

High-Performance Liquid Chromatographic Method for the Analysis of Fluconazole in Pharmaceutical Preparations

INORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE

Drilling Extending Mineralization in La Mina North Zone

Intensive Field Based Exploration Program Commences at Dobsina Cobalt-Nickel-Copper Sulphide Project

Determination of loratadine in pharmaceuticals by a spectrophotometric method

Restricted Substances List

Quality by design (QbD) is an intelligent

An Automated Application Template for Dissolution Studies

Journal of Pharmaceutical and Biomedical Analysis Letters. Analysis Letters

CDER Risk Assessment to Evaluate Potential Risks from the Use of Nanomaterials in Drug Products

Department of Chemistry, Lafayette College, Easton, PA 18042, USA

Ambient Air Sampling Program First Quarter 2016 Report Sudbury, Ontario. Submitted to:

OXFORD CAMBRIDGE AND RSA EXAMINATIONS GCSE B741/01. GATEWAY SCIENCE CHEMISTRY B Chemistry modules C1, C2, C3 (Foundation Tier)

The Danish register for mandatory registration of nanoproducts. Flemming Ingerslev, Section of Chemicals The Danish Environmental Protection Agency

Transcription:

Data Sharing Initiatives Dr Andy Teasdale PQRI/USP Workshop on Implementation Status of ICH Q3D Elemental Impurity Requirements - Analytical and Risk Assessment Challenges

Overview areas covered Why share data? What data already exists? How can this be augmented? What s the strategic intent of the database? Contributing data to the database / current status Vision for how the database could be used to facilitate risk assessments

Why Share Data? ICH Q3D is predicated on the evaluation of risk, this is made of 3 factors RISK = PROBABILITY x Severity x Detectability We know the severity Defined PDEs. We have detectability. DATA either newly generated or Historical data informs us as to the probability. Sharing data thus allows us to make informed judgement during the IDENTIFY and EVALUATE PHASES 3

Why Share Data? Q3D itself comments specifically on this: SECTION 5 - Information for this risk assessment includes but is not limited to: data generated by the applicant, information supplied by drug substance and/or excipient manufacturers and/or data available in published literature. SECTION 5.5. The data that support this risk assessment can come from a number of sources that include, but are not limited to: Prior knowledge; Published literature; Data generated from similar processes; Supplier information or data; Testing of the components of the drug product; Testing of the drug product. 4

Why Share Data? Q3D Case Studies use of first principles approach based on existing data exemplified. 5

What data already exists? How can this be augmented? Container Closure Systems THEORETICAL RISK Especially in the case of liquid formulations there is risk of metals leaching out of CCS into the formulation WHAT DOES THE DATA SAY? Materials in Manufacturing and Packaging Systems as Sources of Elemental Impurities in Packaged Drug Products: A Literature Review PDA J Pharm Sci Technol January/February 2015 69:1-48; Section 5.3 Probability of elemental leaching into solid dosage forms is minimal and does not require further consideration in the risk assessment 6

What data already exists? How can this be augmented? EXCIPIENT STUDIES Study involved: Some 200+ samples Examined 24 elements Summary of results Little evidence of substantial levels of even the big 4/Class 1 (ubiquitous?) in mined excipients Pb seen in TiO2 but levels <10ppm, variability not significant. Pb also seen in Zn Stearate. Cd levels in Magnesium hydroxide / Calcium carbonate exceed Option 1 limits levels need to fail to an option 2 limit before serious concern 7 THIS IS 200 SAMPLES WHAT IF WE COULD COLLATE DATA FROM 2000+ SAMPLES?

What data already exists? How can this be augmented? 8 Potential to facilitate more scientifically driven elemental impurities risk assessments and reduce unnecessary testing as part of the elemental impurities risk assessment efforts. The data to be shared is the analytical data generated to establish the levels of trace metals within batches of excipients used in the manufacture of pharmaceuticals.

What s the strategic intent of the database? Become the primary source of EI data for excipients that drives initial risk assessment (c.f. the Jenke paper for packaging components & EIs) Publish key findings with the intention of de-risking commonly used excipients Compare / contrast with data published generated by FDA. 9

Building the database How has the database been built? How much data is in it? Lhasa designed and developed the Elemental Impurities database based on VITIC TM platform Approved by the consortium in December 2015 Initial round of donations was received beginning of 2016 The database was first released at the end of March 2016 The Elementals database v2016.1.0 contains the following number of records: 52 records in the Excipient table. 123 records in the Elementals table. 10 V2016.2.0 just released now contains 157 excipients 757 result records

Building the database Procedure/process for organizations to share their in-house data Template defined to allow error free parsing of data. Data anomolised and checked by Lhasa. Data quality requirements Extensive discussions relating to data requirements Validation protocol generated 11 Extent of Validation recorded + Digestion Conditions No difference between data donated and data published in peer review journal in terms of vindication of data

Building a database Is all of the data for lactose and how will sufficient diversity of materials and suppliers be managed? The content of the database will be actively managed Clear commitment from members to generate data if gaps are identified Next data release will give a clearer picture to consortia members ListNo CarlMrozListName Total 1 Magnesium stearate 23 2 Microcrystalline cellulose 41 3 Lactose 32 4 Starch 14 5 Cellulose derivatives 18 6 Sucrose 9 7 Povidone 15 8 Stearic acid 3 9 Dibasic calcium phosphate 18 10 Polyethylene glycol 6 Number of results 45 40 35 30 25 20 15 10 5 12 0 1 2 3 4 5 6 7 8 9 10

How is use of the database envisioned? At EMA meeting in April EFPIA presented a series of Case Studies The following slide examines how / where pre-existing data can facilitate the risk assessment 13

Oral Solid Dose Component Functionality Amount per 400 % in coated Type (Excipient) mg tablet (mg) tablet Core API Drug substance 400.00 62.64 Hypromellose 2910 Binder 21.70 3.40 Plant Microcrystalline Diluent Cellulose 37.20 5.83 Plant Lactose Diluent Monohydrate 111.50 17.46 Animal Crospovidone Disintegrant 43.40 6.79 Synthetic Magnesium stearate Lubricant 6.20 0.97 Mineral Coating Hypromellose 2910 Film-former 11.16 1.75 Plant Titanium dioxide Pigment 5.55 0.87 Mineral Triacetin Plasticiser 1.49 0.23 Synthetic Blue Aluminium Lake Colorant #2 0.37 0.06 Mineral Blue Aluminium Lake Colorant #1 0.03 0.005 Mineral Several Excipients used in the formulated product. What data are available? Number of materials FDA External DB Internal Lactose 6 3 Hypromellose 2910 6 (not defined as 2910) MCC 14 6 Crospovidone 17 (povidone) Magnesium Stearate 1 7 9 Titanium Dioxide 7 Blue Aluminium Lake #1 1 Blue Aluminium Lake #2 8 3 Database should contain substantively more data for common excipients Note Lactose is the main excipient others <10%

Excipient data Maximum level seen (ppm) Number of materials As Cd Hg Pb V Ni Co FDA Extern Intern FDA Extern Intern FDA Extern Intern FDA Extern Intern FDA Extern Intern FDA Extern Intern FDA Extern Intern FDA Extern Intern DB DB DB DB DB DB DB DB Lactose 6 3 <0.23 <0.03 <0.08 ND <0.5 ND <0.08 ND <2 ND <3 ND <0.8 ND Hypromellose 2910 6 8 0 <0.03 0 <0.1 0 <0.3 0.01 <0.1 0.02 ND 0.64 2.09 0.01 <1 MCC 14 6 <1.0 ND <0.2 ND <0.5 ND <0.2 <0.1 <2 ND <3 <1 <0.8 ND 0.2 (actual number above LOQ) Crospovidone 17 3 0.02 ND 0 ND 0 ND 0.06 ND 0.02 ND 0.1 ND 0.1 ND Magnesium Stearate Titanium Dioxide Blue Aluminium Lake #1 1 7 9 0.02 <0.23 0.09 0 <0.2 <0.1 0 <0.5 <0.3 0.01 <0.2 <0.1 0 <2 1.7 0.16 <5 1.5 0 <0.8 <1 0.5 (actual number above LOQ) 7 0.36 0.07 0.04 5.74 5.95 0.48 0.04 1 0 0.01 0.03 0.03 0.26 1.58 0.01

Excipient data Reflection on significance No appreciable traces of Class 1 or Class 2a elements in low risk excipients Lactose Povidone MCC Mg Stearate Ni seen at 1.5ppm NB less than 1% of the formulation Titanium dioxide 6ppm Pb / 6ppm V Is this significant? Component Functionality Amount % in coated Type (Excipient) per 400 mg tablet tablet (mg) Core Drug substance API 400.00 62.64 Hypromellose 2910 Binder 21.70 3.40 Plant Microcrystalline Diluent Cellulose 37.20 5.83 Plant Diluent Lactose Monohydrate 111.50 17.46 Animal Crospovidone Disintegrant 43.40 6.79 Synthetic Lubricant Magnesium stearate 6.20 0.97 Mineral Coating Hypromellose 2910 Film-former 11.16 1.75 Plant Titanium dioxide Pigment 5.55 0.87 Mineral Triacetin Plasticiser 1.49 0.23 Synthetic Blue Aluminium Lake Colorant #2 0.37 0.06 Mineral Blue Aluminium Lake Colorant #1 0.03 0.005 Mineral

Excipient data Reflection on significance Component Category Quantity (mg/form) Dose "x" form (mg/day) Arsenic in component As ug in daily dose of Lead in component Pb ug in daily dose of ug/g formulation ug/g formulation Mercury in Hg ug in daily dose of component ug/g formulation Cadmium in Cd ug in daily dose of component ug/g formulation Vanadium in component ug/g V ug in daily dose of formulation Cobalt in component ug/g Co ug in daily dose of formulation Nickel in component Ni ug in daily dose of ug/g formulation x = 1 Total Bio Acc Total Bio Acc Total Bio Acc Total Bio Acc Total Bio Acc Total Bio Acc Total Bio Acc Total Bio Acc Total Bio Acc Total Bio Acc Total Bio Acc Total Bio Acc Total Bio Acc Total Bio Acc Dosage Form : Active Synthetic 400 400 0.00 0.00 0.00 0.0 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 Hypomellose Synthetic 32.9 32.9 0.03 0.00 0.00 0.1 0.00 0.00 0.30 0.01 0.00 0.10 0.00 0.00 0.03 0.00 0.00 1.00 0.03 0.00 2.09 0.07 0.00 MCC Plant derived 37.2 37.2 1.00 0.04 0.00 0.2 0.01 0.00 0.50 0.02 0.00 0.20 0.01 0.00 2.00 0.07 0.00 0.80 0.03 0.00 3.00 0.11 0.00 Lactose Animal 112 112 0.23 0.03 0.00 0.1 0.01 0.00 0.50 0.06 0.00 0.08 0.01 0.00 2.00 0.22 0.00 0.80 0.09 0.00 3.00 0.34 0.00 Crospovidone Synthetic 43.4 43.4 0.02 0.00 0.00 0.1 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.02 0.00 0.00 0.10 0.00 0.00 0.10 0.00 0.00 TiO2 Mineral 5.5 5.5 0.36 0.00 0.00 5.9 0.03 0.00 0.04 0.00 0.00 0.07 0.00 0.00 5.95 0.03 0.00 0.04 0.00 0.00 0.48 0.00 0.00 Mg Stearate Mineral 6.2 6.2 0.23 0.00 0.00 0.2 0.00 0.00 0.50 0.00 0.00 0.20 0.00 0.00 1.70 0.01 0.00 1.00 0.01 0.00 1.50 0.01 0.00 Al Lake 1 Mineral 3 3 0.00 0.00 0.00 0.0 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.01 0.00 0.00 Triacetin Synthetic 1.5 1.5 0.00 0.00 0.00 0.0 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 Al Lake 2 Mineral 0.3 0.3 0.00 0.00 0.00 0.0 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 Total Dosage Form weight 642 642 Total element As 0.07 0.00 Pb 0.06 0.00 Hg 0.09 0.00 Cd 0.02 0.00 V 0.34 0.00 Co 0.16 0.00 Ni 0.53 0.00 Permissible Limits As Pb Hg Cd V Co Ni Formulation Q3D Q3D Q3D Q3D Q3D Q3D Q3D Oral PDE 15 5.0 30 5 100 50 200 Parenteral PDE 15 5.0 3 2 10 5 20 inhaled PDE 2 5.0 1 2 1 3 5 Based on data from database all predicted to be ~1% or less of PDE

Challenges to using first principles The data set is limited! - True but plan to develop a critical mass. Mined excipients will always show variability - Potentially true.. Component Dosage Form : Category Quantity (mg/form) Dose "x" form (mg/day) Arsenic in component ug/g As ug in daily dose of formulation Lead in component ug/g Pb ug in daily dose of formulation x = 1 Total Bio Acc Total Bio Acc Total Bio Acc Total Bio Acc Active Synthetic 400 400 0.00 0.00 0.00 0.0 0.00 0.00 Hypomellose Synthetic 32.9 32.9 0.03 0.00 0.00 0.1 0.00 0.00 MCC Plant derived 37.2 37.2 1.00 0.04 0.00 0.2 0.01 0.00 Lactose Animal 112 112 0.23 0.03 0.00 0.1 0.01 0.00 Crospovidone Synthetic 43.4 43.4 0.02 0.00 0.00 0.1 0.00 0.00 TiO2 Mineral 5.5 5.5 0.36 0.00 0.00 1000.0 5.50 0.00 Mg Stearate Mineral 6.2 6.2 0.23 0.00 0.00 0.2 0.00 0.00 Al Lake 1 Mineral 3 3 0.00 0.00 0.00 0.0 0.00 0.00 Triacetin Synthetic 1.5 1.5 0.00 0.00 0.00 0.0 0.00 0.00 Al Lake 2 Mineral 0.3 0.3 0.00 0.00 0.00 0.0 0.00 0.00 How much impact would this have in the case of an excipient such as TiO2? 1000ppm Pb / Hg? Pb overall just exceeded RISK = PROBABILITY x Severity x Detectability Total Dosage Form weight 642 642 Total element As 0.07 0.00 Pb 5.52 0.00

Next Steps Hear more about the database - December 7 th Join Us! Contact : Crina.Heghes@lhasalimited.org

Conclusions The feasibility of sharing excipient elemental impurity data has been successfully demonstrated. Pooling and publishing data; Can surely help to improve the ease with which risk assessments can be completed Will give a much better picture of which materials represent a more significant risk than others Indicate where the risk is real & where it is negligible Reduce the amount of testing that is needed to be done moving forward to support implementation Confidentiality Notice This file is private and may contain confidential and proprietary information. If you have received this file in error, please notify us and remove it from your system and note that you must not copy, distribute or take any action in reliance on it. Any unauthorized use or disclosure of the contents of this file is not permitted and may be unlawful. AstraZeneca PLC, 1 Francis Crick Avenue, Cambridge Biomedical Campus, Cambridge, CB2 0AA, UK, T: +44(0)203 749 5000, www.astrazeneca.com 20