In Organistry we perform studies in order to identify unknown impurities of API’s caused either by degradation or by interaction with an excipient.
You can send a sample with an impurity (≥ 0.1%) to identify it by HPLC-MSn, and then, we can prepare it by synthesis in order for you to determine its response factor in the analytical method and qualify it.
Under one roof, we cover the analytical and the synthetic areas, allowing us to rapidly resolve the problems associated with the impurities of your products.
We work with more than 20 pharmaceutical companies (manufacturers of active ingredients and formulators) conducting this type of work.
We have a wide experience in identification with several families of products and various types of formulations (tablets, syrups, gels, etc.). Also we identify extractables and leachables that can be contained in pharmaceutical products.
Phases of the process of identification and obtaining your unknown impurity:
HPLC-MSn
Our organic chemists propose structures for your unknown impurity using the information of the API, the excipients and the conditions of impurity generation (including forced degradation studies if available). We carry out bibliographic searches that support our proposals.
Then studies are performed in the HPLC-MS Ion Trap + Orbitrap (MSn; exact mass) of the impurity to identify including MSMS fragmentation to obtain structural information.
If there is consistency with any of the proposed structures we can directly move onto to the synthesis of the impurity, without previous isolation.
If your analytical method were not compatible with MS, we would adapt it previously (using a volatile buffer).
Isolation and characterization
In some cases the study of HPLC-MSn does not allow us to identify your unknown impurity (eg. Due to the existence of isomers).
This problem is solved by isolating the impurity in our preparative HPLC Waters and identifying it by Nuclear Magnetic Resonance (NMR).
For the 1D and 2D-NMR studies, we access to the equipment of Services to Support Research (SAI) of University of A Coruña (UDC) in self-service mode.
Thus, we can offer competitive prices on all our analysis (MS, NMR, EA, FTIR, etc.) and with a short delivery time.
Obtaining impurity
In our organic synthesis laboratory we can prepare your previously identified impurity.
If we can not carry out a directed synthesis or it is not efficient, specific forced degradation experiments are designed to generate the impurity and obtain a standard after its isolation by preparative HPLC.
The impurities are supplied with a certificate of analysis that includes NMR, HPLC, MS, AE, KF and all the analytical data necessary for its complete characterization.
