Pharmaceutical Analysis LABORATORY

Head

Agnieszka Zielińska, M. Sc.

phone +48 601 991 900

agnieszka.zielinska@ichp.lukasiewicz.gov.pl

The Quality Control Section carries out analyses in the field of control:

• starting materials used in the manufacture of active substances and medicinal products
• intermediates manufactured in the production process (in-process testing)
• final products – active substances
• medicinal products
• packaging materials in which active substances are stored
• manufacturing conditions, including cleaning processes of process equipment

according to Ph. Eur., USP, FP under GMP standard.

The scope of the team’s activities also includes:

• stability studies (long-term, accelerated, intermediate) carried out in accordance with the principles laid down in the ICH International Guideline: ‘Stability’ Q1A-Q1F;
• ageing tests of both active substances produced by the Łukasiewicz Research Network – Industrial Chemistry Institute of Industrial and medicinal products commissioned by contractors.
• standardisation of standards for active substances and their impurities used in the various projects carried out at the Institute and offered for commercial purposes

• development and validation of analytical methods in accordance with current ICH requirements.
• transfer of analytical methods
• development and validation of analytical methods for cleaning process equipment used in the manufacture of active substances and medicinal products.
• determination of residual solvents in active substances by classical and Head Space methods.
• pharmaceutical availability studies (release profiles).

On the basis of regular inspections carried out by the Main Pharmaceutical Inspectorate, the Łukasiewicz Research Network – Industrial Chemistry Institute is in possession of Certificates which confirm compliance of production conditions of active substances with the requirements of GMP.

In addition, the Quality Control Section authorised by the GIF to manufacture the Medicinal Product in the scope of manufacturing operations: physicochemical tests in quality control. The team accepts analyses on request using available techniques and after signing the relevant quality agreements.

Research potential:

Research is carried out using high-end apparatus based on a broad spectrum of separation, isolation and identification techniques:

• High-performance liquid chromatography (HPLC, UPLC)
• Gas chromatography (GC-FID, GC-HS)
• Thin-layer chromatography (TLC)
• Infrared spectroscopy IR
• Spectroscopy in ultraviolet and visible light (UV-VIS)
• Instrumental and classical analysis

Head

Anna Chorąży, Eng.

phone +48 668 427 668

anna.chorazy@ichp.lukasiewicz.gov.pl

Łukasiewicz – ICI, Pharmaceutical Analytical Laboratory, Chemical Analysis Section has again been awarded an ISO 9001 compliant Management System Certificate valid until 31.01.2027 as part of a recertification audit

The Chemical Analysis Section carries out analyses of active substances, medicinal products, excipients, pharmaceutical raw materials according to Ph. Eur., USP, FP in accordance with the GMP standard.

Areas of operate

• Development and optimisation of analytical methods
• Validation of analytical methods
• Validation of methods for the determination of residues of substances in the process of cleaning the production line
• Verification of analytical
• Transfer of analytical methods
• Batch certification for GMP compliance (certificate) for quality control of medicinal products, active substances and excipients and raw materials
• Pharmaceutical availability studies for various pharmaceutical forms
• Stability testing of active substances and medicinal products in qualified climate chambers under long-term conditions
• Impurity profile testing – detection, identification and quantification of impurities according to the requirements of pharmacopoeial monographs (USP, Ph. Eur., FP), recommendations of the International Conference on Pharmacopoeia (ICIP), and the International Conference on Pharmacopoeia (ICP). Harmonisation (ICH), the requirements of the European Medicines Agency (EMA) and the US Food and Drug Administration (FDA)
• Standardization of standards for active substances and their impurities.

Research equipment

Research is carried out using high-end apparatus based on a broad spectrum of separation, isolation and identification techniques.

• Liquid chromatography – HPLC (UV/PDA/RI/Fluorescence/Electrochemical) on analytical, preparative and semi-preparative columns, UPLC, SEC, IEC
• Gas chromatography – GC with Headspace and FID detection
• Spectroscopy – IR, NIR, FTIR, UV-VIS
• AAS/AES spectrometry flame and electrothermal excitation
• Analysis of particle distribution, size and shape – laser diffraction, microscopic method
• Potentiometry
• Classical methods: weight analysis, titration analysis

For many years, the Chemical Analysis Section has been cooperating with pharmaceutical companies and research centres in Poland and abroad in the field of quality control of medicinal products and raw materials, development studies, expert opinions and consultancy in the drug registration process.

Head

Marta Zezula, PhD. Sc. Eng.

phone +48 601 333 919

marta.zezula@ichp.lukasiewicz.gov.pl

In the Research Analytics Section, research work is carried out on the full analytical characterisation of chemicals and pharmaceuticals, as well as analytical work for various pharmaceutical forms (tablets, capsules, solutions, eye drops in solution and suspension form, emulsions and ointments). On the basis of the research conducted, documentation is prepared that meets the requirements of the committees creating quality criteria for medicines, including the International Council for Harmonisation of Technical Requirements for Registration of Pharmaceuticals for Human Use (ICH) and the European and US registration authorities.

The Research Analytics team cooperates with scientific and industrial units by carrying out analytical work as part of scientific projects. The results of research work are presented in national and international journals and at scientific conferences.

Areas of operate

Expertise, method development and validation in:

• determination of chemical and enantiomeric purity and content of chemical and pharmaceutical substances (HPLC, UHPLC with UV/VIS detection, PDA, Corona CAD, MS)
• determination of complete contaminant profiles, including genotoxic ones
• determination of release profiles for the active substance(s) in drug form (HPLC, UHPLC with UV/VIS detection, PDA)
• studies on the compatibility of the active substance with excipients at the development stage
• determination of residual solvent content (GC-FID, GC-HS, GC-MS)
• determination of substance content by potentiometric titrations
• determination of trace elements (ICP-MS)
• determination of water content using the volumetric and coulometric Karl Fischer methods,
• chemical structure determination (NMR, IR and Raman spectroscopies, X-ray mono-crystalline and powder diffraction)
• qualitative and quantitative analyses of phase transformations in solids, including polymorphic transformations (e.g. quantitative analysis using the Rietveld method) and calculation of the degree of crystallinity
• determination of particle size and shape distribution profiles
• determination of solubility and determination of pKa (UV-Vis)
• stability studies under accelerated and long-term conditions.

Polymorphism studies

• X-ray powder diffraction (XRPD)
• X-ray monocrystalline diffraction
• differential scanning calorimetry (DSC)
• infrared spectroscopy (FTIR/ATR)
• Raman spectroscopy

Preformulation studies

• laser diffraction
• automated microscopic analysis
• PH solubility test of active substances. Eu.

GMP analyses

• X-ray powder diffraction (XRPD)
• gas chromatography with mass spectrometry detection (GC-MS)
• nuclear magnetic resonance (NMR 500 MHz)
• trace element analysis (ICP-MS)

Drug form analysis

• preformulation testing: solubility testing and release profiles
• physico-chemical tests and pharmaceutical availability tests for different pharmaceutical forms
• analysis of food supplements (identity, content, heavy metals)
• analysis of natural products (identity, content and release) and veterinary products (identity, content, release and chemical purity).

Head

Edyta Pesta, M. Sc.

phone +48 453 056 167

edyta.pesta@ichp.lukasiewicz.gov.pl

The Pharmacokinetics Section works on bioequivalence studies and bioavailability of medicinal products. Since 2003, the team has been working according to the principles of Good Laboratory Practice (Certificate No. 25/2020/DPL). The team has performed more than 400 validations of analytical methods and pharmacokinetic studies in collaboration with national and international pharmaceutical companies and clinical centres.

Areas of operate

• Study design preparation
• Development or adaptation of a bioanalytical method for the determination of a medicinal substance and/or metabolites in biological material
• Validation of the bioanalytical method in accordance with EMA requirements
• Performance of assays in a biological material (HPLC, LC/MS/MS)
• Pharmacokinetic calculations (WinNonlin)
• Study documentation in CTD format Module 5:
• Archiving of biological material samples (≤-14°C and ≤ -60°C)
• Preparation of expert opinions
• Management of pharmacokinetic studies (including clinical part)
• Preparation of application for funding

Research equipment and capacity:

• Quattro PREMIER tandem mass spectrometer (Waters) coupled to HPLC (LC/MS/MS)
• LCMS-2010 mass spectrometer (Shimadzu) coupled to HPLC (LC/MS)
• UHPLC and HPLC with UV-VIS, electrochemical and fluorimetric detectors

• XEVO TQ-XS mass spectrometer connected to an Acquity Class I UPLC

• SOLO Version 8.37 sample preparation machine for analysis, from Hudson Robotics, Inc.
  

• Free online tool for the presentation of Incurred sample reanalysis (ISR) results prepared in collaboration with the Warsaw University of Technology, available at https://modelvis.shinyapps.io/isrVis/. The tool was presented in the journal Bioanalysis, Vol.9, No.12.
• A free online tool to help find the cause of ISR results not meeting acceptance criteria, prepared in collaboration with the Warsaw University of Technology: https://modelvis.shinyapps.io/isr3d/ . The tool was presented in the journal Bioanalysis, Vol.10, No.3

GOOD LABORATORY PRACTICE CERTIFICATE

(GOOD LABORATORY PRACTICE CERTIFICATE)

List of bioanalytical methods in GLP system

Head

Bogna Piątkowska, M. Sc.

phone +48 507 333 379

bogna.piatkowska@ichp.lukasiewicz.gov.pl

The Microbiological Analysis Section carries out microbiological testing work for industrial clients and as part of Łukasiewicz- ICHP’s internal co-operation. The Microbiological Analysis Section is GMP-certified and is regularly audited by contract research companies and the General Pharmaceutical Inspectorate. In addition to standard tests in quality control, the team also develops test methods for specific pharmaceutical and non-drug products.

Areas of operate

• sterility testing
• microbiological purity testing
• testing of bacterial endotoxins (gel method: limit test)
• antimicrobial efficacy testing
• effectiveness of disinfectants
• microbiological monitoring of clean rooms
• testing of the fertility and sterility of microbiological media
• validation and transfer of microbiological methods – confirmation of the suitability of a method for a given application.

Research potential:

• premises of appropriate cleanliness classes, including Class B,
• cabinets with laminar air flow,
• heaters, autoclave, steriliser, water bath, analytical balances, steritest and other necessary equipment for analyses

ISO-9001-253644-2018-AQ-POL-RvA-4-en-PL-20240131-20240131062700 Łukasiewicz Research Network – ICI, Pharmaceutical Analytical Laboratory, Chemical Analysis Section has again received an ISO 9001 compliant Management System Certificate valid until 31.01.2027/ as part of a recertification audit.