Nuclear magnetic resonance spectroscopy (NMR)

 

Utilising both a 600 MHz and 400 MHz instrument we are able to support our clients with problem solving, QC testing and impurity identification

 

RSSL has over 25 years’ experience in the use of NMR as a valuable analytical technique in the life sciences sector and is one of only a few contract laboratories in the UK to offer access to a 600 MHz instrument in a GxP compliant environment, this compliments our 400MHz instrument.

 

The extensive NMR capacity at RSSL allows for the development of novel analytical approaches to solve problems that are not answered by more routine experiments, whilst continuing to provide a reliable, regular service to meet the requirements of various pharmacopeial quality control tests. 

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NMR is a valuable analytical tool with extensive applications which directly observes atoms (nuclear spins) of molecules when detailed molecular information is essential. Its ability to provide both qualitative and quantitative data makes it a key technique, of which both NMR and Quantitative NMR (qNMR) is available at RSSL. NMR (Nuclear Magnetic Resonance) analysis is a powerful spectroscopic technique with a large range of applications within the food and pharmaceutical industry.

 

  • Confirmation of small molecule structures: NMR is an ideal technique for confirming the structure of small molecules. It provides detailed information about the connectivity of atoms within a molecule, which allows chemists to determine the molecular structure without the need for reference materials.
  • Authenticity screening / fraud detection: NMR can be used as a non-targeted approach to screen for authenticity or detect fraudulent products. By comparing NMR spectra of known authentic samples with the unknown samples, discrepancies can be identified, indicating potential adulteration or fraud.
  • Quantitative assessment of purity / assay: NMR provides quantitative data, enabling the assessment of purity and assay of API/novel compounds. This can be done quickly and with minimal method development, without relying on certified reference materials, which can be expensive or challenging to obtain.
  • Structure elucidation of unknown impurities: NMR, in combination with accurate mass LC-MS (Liquid Chromatography-Mass Spectrometry), is invaluable in determining the structures of isolated unknown impurities. The two techniques complement each other and provide a comprehensive analysis of complex samples.
  • Fingerprinting of organic material: NMR can provide a unique fingerprint of organic materials present in a sample. This is particularly useful in cases of suspected fraudulent products or when trying to reverse engineer or de-formulate a product to understand its composition.
  • Versatility with different matrices / dosage types: NMR is versatile and can be applied to a wide range of sample matrices and dosage forms, making it suitable for various applications.
  • Multiple nuclei experiments: NMR is not limited to just proton (1H) and carbon-13 (13C) nuclei. It can be applied to various other nuclei, such as fluorine (19F), phosphorus (31P), and nitrogen (15N). Additionally, 2D (Two-dimensional) correlation experiments provide even more detailed information about the molecular structure and interactions.
  • QC and monograph testing: a common application of the NMR techniques within the pharmaceutical industry, it can also be used however, for research and contamination investigations. 

 

 

Can NMR be quantitative?

 

NMR spectroscopy has traditionally been used for structure elucidation of small molcules, however it can also provide quantitative information, even in complex mixtures, meaning that quantitative NMR (qNMR) has gained a higher degree of importance for the pharmaceutical industry over the years.

 

As an intrinsically linear response is observed by qNMR there is no requirement for a calibration curve or conditioning prior to measurements, making it suitable for automation. This saves time and resources while ensuring accurate quantitative analysis, making it a preferred option over other methods that may require certified reference materials and ideal for high-throughput analysis and urgent projects. 

 

 

 

 

Why choose RSSL for NMR?

 

RSSL's NMR service is fully compliant, meeting Good Manufacturing Practice (GMP) requirements and has been inspected and approved by regulatory bodies like the U.S. Food and Drug Administration (FDA) and the Medicines and Healthcare products Regulatory Agency (MHRA).

 

Both of RSSL's NMR spectrometers are GMP qualified and fully compliant. Our 600MHz magnet provides enhanced resolution NMR spectra, which improves accuracy and confidence in structural elucidation and deformulation projects. These factors, especially in a GMP environment, ensure reliability and traceability of results. 

 

At RSSL we understand the importance of timely results, our NMR runs can be completed under tight time restraints. qNMR also eliminates the need for reference materials of the compound of interest. This saves time and resources while ensuring accurate quantitative analysis, making it a preferred option over other methods that may require certified reference materials. These efficiencies are especially advantageous for high-throughput analysis and urgent projects.

RSSL promotes a collaborative approach within the laboratory, the access to other teams within the organisation brings a wealth of expertise and experience (30 years cross-lab experience) allowing for a comprehensive and thorough analysis of samples. The integration of NMR data with other analytical techniques, such as LC-MS, UV, and FTIR, further enhances the depth of information obtained.

These qualities make RSSL a reliable and valuable partner for NMR-related projects, especially in pharmaceuticals and other regulated industries

Frequently asked questions

  • A major use of NMR in the pharmaceutical industry is for structure confirmation of API’s and impurities. It is also used extensively for pharmacopeia testing of raw ingredients and excipients. NMR spectroscopy can be utilised throughout the lifecycle of a drug product, from the discovery stage through to routine quality control (QC) testing.

  • As a technique, NMR is excellent at giving an overview of the organic components within a sample. Preparation and experiment times are shorter than chromatographic techniques so a great deal of information can be obtained on quick timescales. This makes NMR spectroscopy an invaluable tool for problem solving or de-formulation projects. NMR can provide both quantitative and qualitative information over a range of different sample matrices.

  • Purity of small molecules can be established through qNMR, even when part of a complex mixture. qNMR can be advantageous over traditional chromatographic techniques as there is no requirement for a refence material of the compound of interest. 

  • 1H NMR can be performed on less than 1 mg of a pure API, however for less abundant nuclei such as 13C, more sample is preferable. For other work on more complex sample matrices, where more involved sample preparation is required, we may require more sample. qNMR also only requires a small amount of sample for analysis (as little as 2 mg per replicate). 

  • NMR provides valuable information about the chemical composition including identification of unknown compounds and impurities, making it an essential tool in quality control processes to ensure the safety, efficacy, and consistency of products. The technique is used within routine QC testing to identify unknowns, residual solvents, known impurities and assays. 

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