ANYL 148 |
| Chemiluminescence Nitrogen Detection (CLND) can be used as a complementary technique to conventional UV detection for HPLC separations. CLND selectively determines the amount of nitrogen present in the compound of interest and can be use for quantitative analyses. Using four commercially available, highly pure (>99%), stable chemicals as external reference standards, CLND was used to determine the absolute purity (% w/w) of several nitrogen-containing active pharmaceutical ingredients (API). The performance of the detector was evaluated using a series of 12 highly purified compounds that incorporate a variety of nitrogen levels (from 1 to 4 atoms) and structural arrangements. To determine the applicability for % w/w determination, previously well-characterized batches of 6 different APIs were assayed and the results compared to the certificate of analysis assay values; the results obtained were within 1.0 % of the purity determined by HPLC/UV suggesting that this technique is reproducible and accurate. Day-to-day and intra-day variations in the instrument were also determined: the results demonstrated 8 % relative standard deviation (RSD) for day-to-day variation and < 1.0% RSD for intra-day variation. These results indicate that CLND is useful for the independent purity determination of reference materials for pharmaceutical analyses. |
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General Papers
7:00 PM-9:00 PM, Sunday, 10 September 2006 Moscone Center -- Hall D, Poster
Division of Analytical Chemistry |