Journals / Turkish Journal of Pharmaceutical Sciences / 2008 / Cilt: 5 - Sayı: 3
Feksofenadin hidroklorür'ün farmasötik preparatlarda spektrofotomrtrik ve yüksek performanslı sıvı kromatografik yöntemlerle miktar tayini
- Pages
- 175–189
- DOI
- —
Abstract
Abstract In present study, three new spectrophotometric methods, original UV spectrophotometry, first and second order derivative UV spectrophotometry and a new HPLC method were developed for the determination of fexofenadine HCl (FEX) in pharmaceutical preparations. In original UV spectrophotometry, absorbance were measured at 258.7 nm in the zero order UV spectra of the solution of FEX in methanol-water (1:1) in the range of 220 - 290 nm. In first derivative UV spectrophotometry, dA/dl values were measured at 270.4 nm in the first derivative UV spectra of the solution of FEX in methanol-water (1:1) in the range of 245 - 285 nm (AX= 2 nm). In second derivative UV spectrophotometry d2 A/dI 2 values were measured at 252.84 nm in th second derivative UV spectra of the solution of FEX in methanol-water (1:1) in the range of 245 - 285 nm (AX= 2 nm). Linearity range was found as 100.0 - 1000.0 jjg/mL in all the spectrophotometric method Mean recoveries and the relative standard deviations of the methods were found as 99.55 % and 1.10 % in original UV spectrophotometry, 100.97 % and 1.09 % in first derivative UV spectrophotometry and, 99.25 % and 1.10 % in second derivative UV spectrophotometry respectively. In HPLC method, an isocratic system consisted of an ACE C18 analytical column and a mobile phase composed of methanol - phosphate buffer (pH 3.0, 0.1 M) (95:5, v/v) at a flow rate 1.0 mL/min was used for the optimal chromatographic separation using UV detection at 220 nm. Diflucortolone valerate was used as internal standard. Mean recoveries and the relative standard deviations was found as 100.23 % and 0.54 % in HPLC method. All the methods develope were successfully applied to five tablet formulations commercially available in Turkish drug market and the results were compared statistically with each other.
Özet
Bu çalismada feksofenadin HCl (FEX)’ ün farmasötik preparatlarda miktar tayini igin üg yeni spektrofotometrik yöntem, orijinal UV spektrofotometri, birinci ve ikinci türev spektrofotometri,ve yeni bir YPSK yöntemi geliştirilmiştir. Orijinal UV spektrofotometride; absorbans değerleri, FEX’ in metanol-su (1:1) igerisindeki gozeltilerinin 220-290 nm arahgindaki UV spektrumlarmda 258.7 nm de ölgulmustür. Birinci türev UV spektrofotometride; dA/dl değerleri, FEX’ in metanol-su (1:1) igerisindeki gozeltilerinin 245-285 nm arahgindaki birinci türev UV spektrumlarmda (AX= 2 nm) 270.4 nm de olgulmustür. İkinci türev UV spektrofotometride; ^A/dl 2 değerleri FEX ‘in metanol-su (1:1) igerisindeki gozeltilerinin 245-285 nm arahgindaki ikinci türev UV spektrumlarmda (AX= 2 nm) 252.84 nm de olgulmustür. Her üg spektrofotometrik yöntem igin de dogrusal galisma araligi 100.0 - 1000.0 jjg/mL olarak bulunmuştur. Yöntemlerdeki ortalama geri kazamm ve bagil standart sapma değerleri sırasıyla orijinal UV spektrofotometride % 99.55 ve % 1.10, birinci türev UV spektrofotometride, % 100.97 ve % 1.09 ve ikinci türev UV spektrofotometride % 99.25 ve % 1.10 olarak bulunmuştur. YPSK yönteminde, ACE C18 kolonu, mobil faz olarak 1.0 mL/dk akis hızında metanol - fosfat tamponu (pH 3.0, 0.1 M) (95:5,h/h) ’ ndan oluşan izokratik sistem ve 220 nm de deteksiyon optimal kromatografik şartlar olarak belirlenmiştir. Diflukortolon valerat ig standart olarak segilmi§tir. YPSK yönteminde ortalama geri kazamm ve bagil standart sapma degerleri sırasıyla 100.23 % ve 0.54 % olarak bulunmuştur. Geliştirilen turn yöntemler Türkiye Hag piyasasinda bulunan 5 adet tablet formulasyonuna ba§anyla uygulanmistır. Elde edilen turn sonuglar kendi aralarında istatistiksel olarak karsilaştırılmistır.