News & Events
Update of USP spectrometry chapters
Times are changing and we help you change with them
While we are still busy preparing the implementation of the USP double chapter <232> and <233> for determination of elemental impurities, also all other chapters for analysis of heavy metals in USP39/NF34 have undergone substantial review work and are now effectuated per May 1st, 2016: chapter <730> “Plasma Spectrochemistry” as well as <852> “Atomic Absorption Spectroscopy”.
What has changed?
Overdue revision of <851> with substantial changes for Atomic Absorption Spectroscopy
The long outdated, rather descriptive chapter <851> “Spectrophotometry and Light-Scattering” has been removed and is replaced by separate chapters for the spectroscopic techniques[i], which are
- <852> Atomic Absorption Spectroscopy
- <853> Fluorescence Spectroscopy
- <854> Mid-Infrared Spectroscopy
- <855> Nephelometry, Turbidimetry, and Visual Comparison
- <857> Ultraviolet-Visible Spectroscopy
Each chapter provides acceptance criteria for suitability and is accompanied by a respective “>1000” chapter for best practices (i.e. <1852>, <1853>, <1854>, <1855> and <1857>). The change had been triggered by a stimuli article in the Pharmacopeial Forum[ii] which tried to align the general chapters for spectroscopic methods. Initially published in USP38-NF33 on May 1st, 2015, the chapters have now become applicable with the current USP update[iii]. The increase in information about the technique is accompanied by a detailed description of the tests to be carried out for qualification of instruments as well as validation and verification requirements of the associated methods.
Whereas validation criteria and acceptance criteria are more or less consistent with current practice (see Table 1 for details), the new chapter entails important changes in the practice of verification of monographed methods. It is explicitly still allowed to perform monographed USP-NF methods without validation and only do a verification instead. However, the extent of a verification is now precisely defined and will usually exceed by far the scope of verifications performed in the past: “Verification of compendial AA methods should, at a minimum, include the execution of the validation parameters for specificity, linearity, accuracy, precision, and limit of quantitation, when appropriate, as indicated in Validation.” This means that for verification, all validation parameters except for robustness, range and intermediate precision have to be carried out. In mathematical terms:
Verification = Validation minus intermediate precision minus robustness
Similar changes implemented for ICP-OES/ICP-MS chapter <730>
With the current USP39-NF34 official as of May 1st, the existing Plasma Spectrochemistry chapter <730> has also been completely revised. Whereas the structure is now very similar to that of the other spectroscopy chapters with introduction, qualification requirements, guidance on the procedure and a detailed validation and verification chapter, there are some differences in the details for the validation parameters (refer to Table 1 for a detailed overview). Here also the major change is a well-defined and for most applications substantially increases the scope for verifications of monographed methods.
<730> or <233>? - that is the question
<730> is now the general chapter for plasma Spectrochemistry methods. Thus the question arises whether you have to be in compliance with this chapter, if you want to measure only elemental impurities in your pharmaceutical drug substance or product. According to the responsible spokesperson of the USP, “<233> is dedicated to the measurements of impurities and <730> covers all pharmaceutical applications of ICP and ICP-MS which can include methods for assay of components”. Thus, if only elemental impurities are to be determined, compliance with <233> is sufficient.
How can Solvias help you?
Each monographed analysis by AAS, ICP-OES or ICP-MS from now on has to be preceded by a thorough verification - beyond compliance with a procedural SST. To lower the initial effort, we have prepared an internal document listing the required verification parameters, thus obliterating the need for a separate verification protocol. Once established, routine analysis can then always refer back to the initial verification allowing fast response times.
For non-compendial methods, full compliance with both the AAS and ICP chapters of USP-NF is only possible after full method validation. This may be achieved by supplementing our generic validations with additional validation/verification experiments. In many cases, full product specific method validations will be indicated.
Please contact your Solvias business developer for details.
Download the PDF for all details including Table 1 and references.