Structural Analysis of Impurities in Pharmaceuticals Using Trap-Free 2D HPLC and the LCMSTM-9030

Introduction

Management and confirmation of the type, quantity, and safety of trace impurities contained in products are important points for ensuring the quality of products in a wide variety of fields including pharmaceuticals (raw materials, final pharmaceutical agents, and generic drugs), foods (health foods and supplements), and fine chemical products (solvents, paints, surfactants, and various chemical products). In terms of impurities in products, known component checks are performed via the HPLC-UV method in quality control departments. Conversely, the measurement and analysis of unknown components using mass spectrometers, which provide better sensitivity and excellent specificity, based on the HPLC-UV method, are requirements in research departments. However, it is not possible to apply the nonvolatile mobile phase conditions used with HPLC as is in LC/MS analysis. Accordingly, in research departments, these are replaced by volatile mobile phase conditions, which is a very labor intensive process. These condition changes carry significant risks regarding changes to the elution order, and the omission of impurities eluted in the vicinity of main components, so very careful investigations are required. This report introduces an example of the structural analysis in which impurities detected under nonvolatile mobile phase conditions were converted into volatile mobile phase conditions on-line without any complicated examination using a trap free 2-dimensional(2D) HPLC, and then subjected to precision mass spectrometry using the LCMS-9030 quadrupole time-of-flight mass spectrometer.

March 22, 2019 GMT