The Analytical Apparatuses available in SERICHIM allow its experienced analytical researchers to detect, quantify and isolate the entire spectrum of organic compounds, which are generated in a chemical reaction.
Detection and quantitation are performed through chromatographic and spectroscopic technique (Mass Spectroscopy, Nuclear Magnetic Resonance, FT- Infrared spectroscopy and UV spectroscopy), while isolation and purification of drug impurities can be obtained with Preparative HPLC and Flash Chromatography.
Summarising, the analytical apparatuses available in the centre to satisfy our customers’ needs are:

  • 1 NMR 400 MHz
  • 1 GC-MS (EI, CI)
  • 1 HS-GC-MS
  • 4 GC
  • 4 HPLC (DAD, RI detectors)
  • 1 FT-IR
  • 2 UV-Vis
  • 1 TLC scanner
  • 1 HPLC preparativo
  • 1 DSC

The network with other referenced private laboratories and Universities allows SERICHIM to access other analytical techniques not available in home. 

Structural Characterisation of impurities

Organic impurities in active substances are to be reported, identified wherever possible, and qualified as indicated, in Pharmacopeiae or in ICH guidelines. Therefore, identification through structural characterisation of impurities is of primary importance in the development of an API, either if the impurities are synthesis-related or if those are degradation products.
Liquid chromatography–mass spectrometry (LC/MS) or gas chromatography-mass spectrometry (GC/MS) methods have high selectivity and sensitivity. Full scan and product ion scan analysis, providing molecular weight information and fragmentation data, respectively, offer rich structural information and allow proposal of candidate structures rather quickly. Afterwards, detailed spectra analysis from NMR spectroscopy correlation techniques (COSY, HSQC, TOCSY, etc.) allows to confirm the molecular structure of an organic impuritiy.
In SERICHIM impurities characterisation can be performed, using HPLC/DAD/MS or GC/MS methods for obtaining molecular weight information and, after isolation of the impurity and purification, using FT-IR spectroscopy for identification of functional groups and NMR spectroscopy for structure confirmation.

Preparation of reference substances

The availability of well-characterized reference substances is essential for carrying out qualitative or accurate quantitative analysis. In fact, most of analytical techniques used in quantitative analysis are comparative rather than absolute (i.e. in an analytical procedure to quantify the amount of a substance present in a sample, the response of the substance of interest is compared with that of a reference material preparation of the same substance). Many times the substance of interest is not commercially available and so, it must be prepared.
Two possible approaches can be followed in this case: to synthesize the compound with the higher degree of purity suitable for the purpose, or, as in the most frequent cases, to isolate it from a matrix where it is present, also in small amount.
In the latter case, the availability of skilled researchers on Preparative HPLC or Flash Chromatography techniques may be the faster and economically more convenient way to fix the issue.
In SERICHIM, either Prep-HPLC or Flash Chromatography apparatuses are available, as well as the necessary expertise to provide a comprehensive service of isolation, purification, characterization of reference substances, packaging of weighed quantities in appropriate containers. A Certificate of Analysis, with Assignment of Potency, is issued for each reference substance prepared.

Analytical Methods Development and Validation

To test a specific characteristic of a substance against established acceptance criteria for that characteristic, an Analytical Method has to be developed, choosing suitable analytical apparatuses and procedures, based on the intended purpose and scope of the analytical method. Method development is a continuous process that progresses with the phase of drug development, requiring different endeavours from the initial to the late phase.
Method Validation is the process of documenting or proving that the Analytical Method developed provides analytical data for the intended use. This activity is generally required for assuring product quality and for achieving acceptance of products by the international agencies (US FDA, PIC/S, WHO, etc.).
Methods are developed and validated for Quality Control of starting materials, intermediates and APIs.
In SERICHIM analytical methods are validated following ICH guidelines, preparing initial validation protocols to submit to the customer for approval, studying Precision/Reproducibility, Accuracy, Linearity, Specificity/Selectivity, Limit of detection, Limit of quantitation,  Robustness / Ruggedness of the developed method and reporting the results of the validation study.
SERICHIM with its experienced analytical researchers is specialized in Analytical Method Development and Validation from early to late stage of an API development processes, refining and expanding the analytical data set in function of the project progresses.
Our analytical services include also:

  • Forced degradation study
  • Chiral method development
  • Solubility (aqueous and non-aqueous)
  • Spectroscopic characterization (MS, NMR, IR, UV)
  • Potentiometric titrations
  • Melting range measure
  • Boiling point measure
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