Determination of fluoride impurities in Leuprolide. Comparison of analytical methods

Robert Lipka , Marta Sobczak , Stanisław Kuś , Sławomir Oszwałdowski , Maciej Jarosz


Fluoride impurities were determined in technical samples of Leuprolide (anti-cancer drug for prosthetic cancer) using reverse-phase liquid chromatography and derivative spectrophotometry. The chromatographic method was based on the ternary fluoride complex with zirconium(IV) and 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol (5-Br-PADAP). The analysis was performed on a Nucleosil C18 column with LiChrosphere RP-100 end-capped phase, using as eluent acetonitrile (85\%v/v) water mixture at pH 4.1±0.2. Fluoride content was determined with use of the method of standard additions (MOSA) as 2.34 mg g−1 and 0.29 mg g−1 in two different samples. A spectrophotometric determination has been carried out by La(III)-F−-ALC [ternary complex La(III)-F−-alizarin complexone] method with using third derivative spectrophotometry. By this method fluoride content was determined as 1.99 mg g−1 and 0.34 mg g−1 in the samples previously analyzed chromatographically. A validation for both (i.e. chromatographic and spectrophotometric) methods was performed. Statistical analysis showed that spectrophotometric methods could not be used for quantitative determination of fluoride in samples containing them in concentration less than 0.5 mg g−1.
Author Robert Lipka - [Politechnika Warszawska]
Robert Lipka,,
, Marta Sobczak - [Warsaw University of Technology (PW)]
Marta Sobczak,,
- Politechnika Warszawska
, Stanisław Kuś (FC / CAC)
Stanisław Kuś,,
- Chair Of Analytical Chemistry
, Sławomir Oszwałdowski (FC / CAC)
Sławomir Oszwałdowski,,
- Chair Of Analytical Chemistry
, Maciej Jarosz (FC / CAC)
Maciej Jarosz,,
- Chair Of Analytical Chemistry
Journal seriesMicrochemical Journal, ISSN 0026-265X
Issue year2000
Keywords in EnglishDerivative spectrophotometry, Fluoride determination, Leuprolide (Leuprorelin), Reversed-phase liquid chromatography, Validation of analytical methods
ASJC Classification1607 Spectroscopy; 1602 Analytical Chemistry
Score (nominal)30
Score sourcejournalList
Publication indicators Scopus Citations = 16; WoS Citations = 16; GS Citations = 19.0; Scopus SNIP (Source Normalised Impact per Paper): 2014 = 1.336; WoS Impact Factor: 2006 = 1.558 (2) - 2007=1.932 (5)
Citation count*19 (2016-05-30)
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