Pharmceutical analysis at WESSLING

Test for sterility using two insulators according to Ph. Eur. 2.6.1

• Membrane filtration method
• Direct feeding method
• Testing with special test systems
• Testing of large-volume samples
• Media additives
• Subsequent growth control, per germ
• Identification of germs with positive results
• Testing of cytostatic agents
• Transmission of intermediate results

Validation of sterility testing

• Preparation of a validation plan/report
• Validation according to Ph. Eur. with 6 test germs
• Method devlopment

Endotoxin tests according to Ph. Eur. 2.6.14

• By Limulus amoebocyte test (LAL test)
• Gel formation limit value method / gel clot (method A, limit test)
• Kinetic turbidimetric method (Method C, quantitative determination)
• Recombinate endotoxin determination (quantitative determination): preserves the natural occurrence of horseshoe crab, since no lysate is used

Determination of bacterial count (bioburden) according to Ph. Eur. 2.6.12

• Total aerobic microbial count (TAMC)
• Total combined yeasts/mould count (TYMC)

Detection of specified microorganisms according to Ph. Eur. 2.6.13

• Quantitative and qualitative detection

Testing for adequate preservation (KBT) according to Ph. Eur. 5.1.3

Combined tests for ready-to-use pharmaceuticals according to Ph. Eur. 5.1.4

Combined tests of herbal medicinal products for oral use according to Ph. Eur. 5.1.8 according to categories A, B, C

Microbiological hygiene monitoring and particle monitoring

• Sampling by qualified WESSLING employees on request
• Provision of contact plates, air sampler and particle measuring device
• Evaluation of contact plates: aerobic bacterial count, yeasts / moulds, enterobacteriaceae
• Surface inspection by means of swabs
• Airborne germ measurements: germ count and moulds
• Particle measurements

Microbiological determination of the value of antimicrobial agents (e.g. neomycin, gentamycin)

Identification of germs

• Biochemical identification of germs using API
• Using Maldi-TOF/MS
• Creation of house germ databases

Testing of raw materials, ancillary and active substances

• Identification and determination of APIs and ingredients
• Quality control of raw materials
• Tests for identity, content and purity according to current national and international monographs or customer regulations (Ph. Eur, USP, JP, RuP, ChP, etc.)

Release tests  

EU-Batch Release Service, including batch release by WESSLING-QP

Stability tests

We conduct long-term, short-term and in-use stability tests on ready-to-use pharmaceuticals, medical products containing pharmaceutical ingredients and active ingredients in accordance with current ICH and GMP specifications. The test includes the parameters relevant for stability, such as content, purity and active substance release.

Our service includes the development of test plans, overview tables for stability tests and individual stability reports.    

Storage without commissioning analytical tests is also possible.   

We can offer you the following climatic conditions:

• 25°C/60% rel. humidity
• 30°C/75% rel. humidity
• 40°C/75% rel. humidity
• Photo stabilities
• Subtropical and tropical conditions on request

Method development, -transfer and -validation

Our pharmaceutical experts at WESSLING develop and validate methods under GMP on behalf of customers. The suitability and thus the validity of all test methods used must be proven during the approval and registration of medicinal products.
In addition, for food and dietary supplements we provide adapted validations based on pharmaceutical validation.

• Development of new and optimisation of existing methods
• Validiation in compliance with ICH guidelines
• Preparation of validation plans
• Preparation of validation protocols and non-confomrance reports
• Preparation of final validation reports
• Method transfer
• Development of test regulations

Elemental impurities - ICH Q3D

The experts for pharmaceutical analysis competently support their customers in implementing the ICH Q3D Guideline, evaluating their active ingredients, reagents, starting materials and excipients and preparing risk analyses.

The elements are determined in our GMP laboratories using ICP-MS and ICP-OES devices.

These techniques have now found their way into international pharmacopoeias. In the European Pharmacopoeia they are listed in chapters 2.2.58 and 2.2.57, in the USP in chapter '233'. Both methods are characterised by the highest selectivity and lowest detection limits.

Our experts at WESSLING are also happy to conduct the product-specific validation of the methods according to the ICH Q2B Guideline.

• Laser diffractometry, EP 2.9.31: determination of particle size
• IR-microscopy (transmission / reflection / ATR): testing for drug authenticity / drug counterfeits, analysis of film thickness
• Characterisation of nanomaterials in ready-to-use medicinal products
• Spectroscopy / spectrometry: IR spectroscopy, UV-VIs spectroscopy, mass spectrometry, mass spectrometry with inductively coupled plasma (ICP-MS/OES)
• Thin layer chromatography: identity testing, semiquantitative purity tests, quantitative purity tests, content determinations
• Gas chromatography (GC, GC-MS): content determination / determination of RLM, identity checks, detectors: DAD, MS, TCD, feed systems: head space and split / splitless
• Liquid chromatography (HPLC, HPLC-MS): content determination, testing for related substances, identity checks, detectors: fluorescence, DAD, UV/Vis, MS, RI
• Sterility tests using two isolators
• Endotoxin determinations, method A and C
• Test for absence of THC
• Paper chromatography
• Determination of total organic carbon (TOC)
• Clarity and opalescence of liquids
• Colouring of liquids
• Conductivity
• pH value: potentiometric method, indicator method
• Relative density
• Drying loss
• Potentiometric titration
• Optical rotation
• Viscosity (rotational viscometry)
• Brookfield viscosity
• Refractive index
• Melting temperature
• Boiling temperature
• Distillation area

Identity testing of pharmaceuticals   

• Ions and functional groups
• Fatty oils by thin-layer chromatography
• Phenothiazines by thin layer chromatography

Limit tests for pharmaceuticals

• Ammonium
• Arsenic
• Calcium
• Chloride
• Magnesium
• Heavy metals
• Iron
• Phosphate
• Potassium
• Sulfate
• Ash/sulphated ash
• Free formaldehyde
• Alkaline reacting substances in fatty oils
• Determination of metal residues
• Testing of fatty oils for foreign oils by thin layer chromatography
• Fatty acid composition
• Sterols in fatty oils
• Determination of solvent residues

Determination of the content of pharmaceuticals

• Acid value
• Ester value
• Hydroxyl number
• Iodine number
• Peroxide number
• Saponification number
• unsaponifiable parts
• Complexometric titration
• Karl Fischer method
• Phenol in sera and vaccines
• Protein in polysaccharide vaccines
• Nucleic acids in polysaccharide vaccines
• Phosphorus in polysaccharide vaccines
• Protein content

Methods of pharmacognosy

• Ash insoluble in hydrochloric acid
• Foreign components
• Stomata Index
• Source number
• Pesticides
• Determination of tannin content in herbal drugs
• Bitter value
• Dry residue and drying loss of extracts
• Aflatoxins B1 in herbal drugs
• Analysis for aistolochic acids in herbal drugs
• Ochratoxin in herbal drugs
• Microscopic examination of herbal drugs

Methods of pharmaceutical technology

• Decay time of tablets and capsules
• Decay time of suppositories and vaginal suppositories
• Drug release from solid dosage forms by dissolution tester (on-/offline)[Paddle and Basket]
• Compilation of release profiles (PMP/EWP/QWP/1401/98), compilation of bioequivalence studies, biowaver
• Friability (abrasion)
• Tablet hardness
• Uniformity of content and mass of single-dose dosage forms
• Visible particles
• Particle size distribution
• Particle contamination - invisible particles
• Determination of the extractable volume of parenteralia
• Ethanol content
• Methanol and 2-propanol
• Microscopy

At WESSLING, the thrust of our analysis and consulting for pharmaceuticals and medical products along with our service portfolio is international. This can be observed firstly in the close cooperation between our experts at the Budapest and Münster sites.  WESSLING is therefore also a partner to pharmaceutical manufactures whose markets lie outside of Europe:

• Both laboratories in Münster and Budapest work according to GMP standards
• Both pharmaceutical sites hold a manufacturing permit according to Section 13 of the German Pharmaceuticals Act (AMG) and an EU import permit
• Our pharmaceutical laboratory in Münster is inspected by the FDA (Food and Drug Administration). As a result, we are also an analysis partner to customers who are operating in the US market
• The close cooperation between our two sites means combined capacities and know-how for our customers, resulting in on-time processing - even of larger orders or those for express analysis

One-stop shop: from us, manufacturers of pharmaceuticals and medical products obtain all laboratory analyses from a single source: microbiology, chemistry and consulting. Thanks to the close integration of our laboratory analysis and consulting, WESSLING is your full-service provider:

Analysis:

• Testing of all dosage forms: testing of sterile and non-sterile solid, semi-solid and liquid pharmaceuticals
• Testing of cytostatic drugs and permit for handling narcotic drugs according to Section 3 of the German Narcotic Drugs Act (BtMG)
• Sterility tests using two isolators: redundancy minimises the risk of failure and thus guarantees that your orders are processed on time
• Determination of elementary contamination by means of ICP-MS/OES

Special analysis:

• Wealth of experience and know-how in developing and validating analytical methods (HPLC, dissolution, GC)
• Approval analyses with subsequent market release by experienced WESSLING QPs (Qualified Person) and logistics solutions
• Close integration of analysis and consulting

70 experts in Budapest and Münster work with the latest technical equipment in equally cutting-edge, generously sized facilities; our laboratory in Münster covers a total floor space of around 1000 square metres

Our pharmaceutical analysis equipment:

• Approximately 20 HPLCs with UV/VIS, DAD, fluorescence, RI or MS detector
• 2 uHPLCs
• 3 gas chromatographs with head space and trap unit, FID or MS detector
• 3 ICP-MS and 1 ICP-OES
• 10 dissolution testers (UV on-/off-line), paddle and basket
• 2 disintegrators
• FT-IR spectometry with ATR unit
• UV/VIS spectometry
• Polarimetry
• Density measuring unit
• Automatic titration unit
• TOC
• Particle size distribution (Malvern)
• 2 endotoxin readers: fluorescence and recombinant measurement
• 2 sterile test isolators with fast-action sluices