April 11, 2017 | News & Notices Effective Analysis of Elemental Impurities
in Pharmaceuticals Using EDX Fluorescence Spectrometry
Release of the Pharmaceuticals Impurities Analysis Method Package

Pharmaceutical Elemental Impurities Analysis System for EDX-7000

Shimadzu Corporation has released the pharmaceuticals impurities analysis method package as a solution for use with its EDX-7000 energy dispersive X-ray fluorescence spectrometer. This package is suitable for the analysis of elemental impurities in pharmaceuticals.

This package contains conditions for two methods. This enables the efficient analysis of a total of 12 elements, including palladium, which is utilized in catalysts, and highly toxic elements, such as cadmium, lead, and arsenic, which are among the 24 elements subject to risk assessment in the guideline related to the management of elemental impurities (ICH Q3D) shared by Japan, the USA, and Europe. Combining this package with the EDX-7000, which is capable of nondestructive analysis without the need for chemical pretreatment, simplifies elemental impurities analysis.

Background to the Development

In recent years, risk assessment for impurities contained in pharmaceutical raw materials has become important. In December 2014, the Guideline for Elemental Impurities (Q3D) was issued by the International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use (ICH). This guideline will apply to new medicines submitted for approval after April 1, 2017, and is also expected to apply to existing pharmaceuticals starting on January 1, 2018. This guideline stipulates that in pharmaceutical formulation, residual quantities of a total of 24 elements, separated into four classes according to their toxicity, must be controlled within permissible limits. High-sensitivity ICP atomic emission spectrometers (ICP-AES) and ICP mass spectrometers (ICP-MS) are utilized for the precision analysis of such elemental impurities. An increasing number of new drug manufacturers and drug substance manufacturers are considering the introduction of energy dispersive X-ray fluorescence (EDXRF) spectrometers in combination with these instruments. EDX systems can measure elemental concentrations nondestructively, and without the need for chemical pretreatment.

In this context, Shimadzu is promoting the full-scale deployment of EDX systems in the pharmaceutical industry. To ensure that users who have purchased an EDX spectrometer can quickly put it to use, Shimadzu has developed the optimal methods for the most important 12 elements to analyze, and has marketed them as a package.


Analysis with the EDX-7000 can be started by putting the sample in the special container and placing it in the instrument. There is no need to chemically pretreat the sample. Special gases and vacuum conditions are unnecessary, and since it operates on household power supply, installation is easy. In addition, by incorporating two kinds of optimized analysis methods in the pharmaceuticals impurities analysis method package, a total of 12 elements*, seven identified as Class 1 and Class 2A, and five from Class 2B as stipulated by the ICH Q3D, can be analyzed effectively. This is also effective for cross checks with other instruments, such as ICP-AES.

  • *: The elements are cadmium, lead, arsenic, mercury, cobalt, vanadium, nickel, palladium, iridium, rhodium, ruthenium, and platinum.

Advantages of Combining the EDX with the ICP-AES and ICP-MS

In addition to EDX systems, Shimadzu offers ICP-AES and ICP-MS instruments. Whereas EDX spectrometers can be used for the analysis of powdered formulations, which are often utilized in oral drugs, ICP-AES and ICP-MS systems are utilized for the analysis of parenteral, inhalants, and solution formulations, which require the detection of ultra-trace components. Combining these techniques can improve operational efficiency. The standard samples used by the pharmaceuticals impurities analysis method package are the same as for the ICP-AES and ICP-MS, so equipment calibration, validity checks as the equipment management issues are straightforward.

Structure of the pharmaceutical impurities analysis method package: Analysis method conditions media and an electronic instruction manual