Table 3 – Detection limits of the MIC-ICP-MS method for USP <232> elements*
The Multiwave PRO microwave reaction system is a powerful tool to assist with full compliance to USP <232> and <233> require- ments, offering:
• Closed-vessel digestion
• Simultaneous high-temperature and high-pressure capabilities that ensure total digestion of all sample types
• Special applications such as microwave- induced oxygen combustion that enable total mineralization of even the most challenging sample matrices, independent of structure and chemical composition.
*Calculated for aspirin C, n = 10; compared to the required specifications in µg/g.
Detection limits:
MIC-ICP-MS procedure The detection limits (DL) of the MIC-ICP-MS method are shown in Table 3 (calculated from 3σ of the digestion blank; n = 10).
Conclusion Upon evaluation from independent parties, closed-vessel microwave-induced oxygen combustion combined with ICP-MS mea- surement (MIC-ICP-MS) is proven as an effective assay of elemental impurities in pharmaceutical products, as demonstrated on enteric-coated aspirin samples of various brands. Complete decomposition of organic matrices—independent of their structure and functional groups—resulted in superior recov- ery data and detection limits when compared to legacy preparation techniques and other closed-vessel digestion techniques.
The coupled MIC-ICP-MS technique provided spike recovery data between 86% and 112% for the Class 1 and Class 2 elements, exceeding the requirements proposed in USP <232> (recovery between 80% and 150%). Detection limits also meet the USP <232> criteria.
To further assist pharmaceutical companies preparing for USP Chapters <232> and <233>, Anton Paar also offers the Pharma Qualification Package (PQP), an extensive instrument Installation Qualification documentation folder. The PQP complies with pharmaceutical regulations such as GMP, 21 CFR Part 11, GAMP- 5, and USP Chapter <1058>, and follows the 4Q model—DQ, IQ, OQ, and PQ (design qualification, installation qualification, operational qualifica- tion, and performance qualification). The PQP documentation package for the Multiwave PRO contains a traceability list, risk analysis, user Standard Operating Procedures (SOPs), as well as a protocol for 21 CFR Part 11 compliance (related to software functionalities such as audit trail and e-signature).
References
1. U.S. Pharmacopeial Convention; http://
www.usp.org/usp-nf/official-text/revision- bulletins/elemental-impurities-limits-and- elemental-impurities-procedures-0.
2. Nam, K.H.; Isensee, R. et al. Spectroscopy 2011, 26(4), 2–7.
Reynhardt Klopper is Product Specialist, and Eric Fox is National Sales Manager, Analytical and Synthetic Chemistry, Anton Paar USA, Inc., 10215 Timber Ridge Dr., Ashland, VA 23005, U.S.A.; tel.: 804-550-1051, ext. 135; fax: 804-550- 1057; e-mail:
eric.fox@
anton-paar.com.
AMERICAN LABORATORY • 25 • JUNE/JULY 2013
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