« SEPARATIONS AND PURIFICATIONS guidelines.5-7 Specifi city, linearity, repeatability, limit of detection,
limit of quantitation, and system precision were evaluated as part of the generic method validation with a pre-set acceptance criterion. In addition, long-term solution stability was assessed to enable the extended use of standards. The accuracy of a generic method for new pharmaceutical compounds is evaluated during the product-specifi c validation and is not included in the discussions below.
Specifi city
Diluent was assessed for potential spectral interference at characteristic emission wavelengths for each element. Spectral interference from a diluent blank can impact the quantitation limit of elements and occasionally result in a false positive. The results in Table 3 show that there is minimal spectral interference from the diluent blank, and the selected wavelengths are distinct for each element.
Linearity
Linearity of a method enables the determination of the dynamic range of the method. The detector response is linear within this range and hence refl ective of the level present in the sample. Quantitation of elements within the dynamic range ensures the detector response is proportional to the concentration present in the sample. Linearity of the method was assessed for each element at primary and
Element Ni Ni
Cu Cu Zn Zn Fe Fe
Mg Mg Sn Sn Pd Pd Pt Pt
Ru Ru
Table 3. Specifi city of Blank Diluent 2% HCl Wavelength (nm)
231.604 232.003 324.752 327.393 206.200 213.857 238.204 239.562 285.213 279.077 235.485 283.998 340.458 363.470 265.945 214.423 240.272 349.894
Blank (n = 3) -0.00 -0.00 0.00 -0.00 -0.02 -0.02 -0.00 -0.00 -0.00 -0.00 -0.01 0.00 0.01 -0.06 -0.00 -0.00 -0.00 -0.00
secondary wavelengths using standards ranging from 0.05 ppm to 50.0 ppm. Assessing specifi city at dual wavelength provides an
Using USP 735 As An Alternative to USP 232/233 for Elemental Impurity Analysis in Pharmaceutical Products
With new USP regulations for elemental impurity analysis becoming enforceable in late 2015, many laboratories are getting prepared to fulfil these requirements. This webinar will discuss one alternative approach to elemental impurity analysis that meets the requirements of sensitivity and repeatability with very little sample preparation.
In this webinar you will learn: • What is USP <735>?
• How it can be an alternative to USP <233>, along with benefits and disadvantages of both
• How to determine if this technique can be used in your laboratory to meet the sensitivity guidelines outlined in USP <232>
View On-demand at:
http://bit.ly/1FnClk6 Speakers: Daniel Davis
Elemental Analysis Product Manager Shimadzu Scientific Instruments
Dan Davis is the Elemental Spectroscopy Product Manager for Shimadzu Scientific Instruments. He received a B.S. degree in Chemistry from Towson State University. He is responsible for managing the elemental spectroscopy products in North & Central America for Shimadzu including: ICP Emission systems, Atomic Absorption systems, X-Ray Fluorescence & Diffraction systems, and Total Organic Carbon analyzers. He has more than 12 years of experience in the industry and contributes to ASTM and Standards Methods through review and submission of analytical methods.
Justin Masone
Elemental Analysis Product Specialist Elemental Spectroscopy Group, Shimadzu Scientific Instruments
Justin Masone is a Product Specialist in the Elemental Spectroscopy Group at Shimadzu Scientific Instruments. He received a B.A. degree in Chemistry from Johns Hopkins University. He is an experienced chemist in the field of elemental analysis, and his work at Shimadzu is focused on supporting ICP Emission systems, Atomic Absorption systems, X-Ray Fluorescence & Diffraction systems, and Total Organic Carbon analyzers.
www.americanpharmaceuticalreview.com |
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