A high proportion of our projects fall under this banner. We are used to developing methods for novel API’s and formulations and carrying out work to meet Regulatory submission requirements.
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Metals testing for pharmaceutical and other products
Industry regulations for testing for heavy metals in products have been changing over the last few years, and Agenda1 has been developing methods to meet these changes.
The changes have moved the industry from outdated colorimetric limits to new quantitative instrument based approaches, principally Inductively Coupled Plasma methods.
The method changes were sign posted and introduced back in 2011, and (via slightly different tracks) have been brought in by both the Ph. Eur and the USP Pharmacopoeia. The USP covers this in two monographs: Elemental Impurities and Limits and Elemental Impurities (USP 232 & 233). These changes came in force in 2013.
USP 232 outlines the recommended limits for fifteen elemental impurities in drug products. Minimally, quantitative analysis should be conducted on Arsenic, Cadmium, Mercury and Lead. Limit values are given as an example based on a daily dose of 10g, therefore formulation specific limits can be developed and applied as required. USP 233 outlines the structure for the analysis of elemental impurities by ICP-OES.
Agenda1 has seen an increase in the number of customers requesting this service and offers GMP Metals Determination by ICP-OES within its MHRA-certified UK laboratory (www.agenda1.co.uk).
Agenda1 has years of experience developing and delivering GMP Quantitative Metals Determination by ICP-OES, in Accordance with USP 232/233, to our clients. This can range from the USP minimum four element analysis, to the full analysis of all elemental impurities suggested in USP 232.
For the analysis in accordance with USP 233, the instrument will be calibrated, typically, between zero and twice the target level of the
elements to be analysed. This calibration will include standardization solutions at 0.5 and 1.5J of the target level. The samples for analysis will be digested in a suitable manner and then analysed alongside a negative control, and a positive control spiked at
the target level for each element. For Mercury analysis, a suitable stabiliser is used.
The EP primary guidance is in line with ICH Q3D guidelines, and is detailed in the EP chapter 2.4.20. The EP changes will be implemented for the 9th Edition and will therefore come into force from the beginning of 2018 when the test for heavy metals will be removed from all individual monographs on substances for pharmaceutical use excluding veterinary substances.
Both pharmacopeia recommend the use of ICP following Microwave Digestion, and such recommendation is usually a technical requirement to achieve the analysis.
We have developed a wide range of ICP-OES methods for the detection of metals in both active and other ingredients used in the manufacturing of pharmaceutical products. We also carry out routine release testing of raw materials for a number of Contract Manufacturing Organizations.