Determination of fluoride impurities in Leuprolide. Comparison of analytical methods
Robert Lipka , Marta Sobczak , Stanisław Kuś , Sławomir Oszwałdowski , Maciej Jarosz
AbstractFluoride 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.
|Journal series||Microchemical Journal, ISSN 0026-265X|
|Keywords in English||Derivative spectrophotometry, Fluoride determination, Leuprolide (Leuprorelin), Reversed-phase liquid chromatography, Validation of analytical methods|
|Publication indicators||= 16; = 16; = 19.0; : 2014 = 1.336; : 2006 = 1.558 (2) - 2007=1.932 (5)|
|Citation count*||19 (2016-05-30)|
* presented citation count is obtained through Internet information analysis and it is close to the number calculated by the Publish or Perish system.