Bazı ilaç etken maddelerin tayini için türev spektrofotometrik yöntem geliştirilmesi
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Dosyalar
Tarih
2014-03-14
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Yayıncı
Selçuk Üniversitesi Fen Bilimleri Enstitüsü
Erişim Hakkı
info:eu-repo/semantics/openAccess
Özet
Tez kapsamında; amlodipin ve valsartanı tek başına içeren ve amlodipin besilat ve valsartan'ı birlikte içeren preparatlarda etken madde miktar tayinleri için spektrofotometrik yöntemler önerilmiştir. Sadece amlodipin ve sadece valsartanı içeren preparatlarda etken madde miktar tayini için doğrudan UV spektrofotometri ve birinci türev UV spektrofotometri önerilmiştir. Doğrudan UV spektrofotometrede amlodipin besilatın standart ve numunelerinin metanoldeki çözeltilerinin 237,3 ve 360 nm'deki, valsartanın ise 249 nm'deki absorbans değerleri ölçülmüştür. Ölçülen bu değerlerde kalibrasyon grafiği çizme ve standart ekleme teknikleriyle etken madde miktar tayini yapılmıştır. Korelâsyon katsayıları, kalibrasyon grafiği çizme tekniğinde amlodipin besilat için 0,9994 ve 0,9960, valsartan için 0,9997; standart ekleme tekniğinde ise amlodipin besilat için 1,0000 ve 0,9962 ve valsartan için ise 0,9989 olarak hesaplanmıştır. Birinci türev UV spektrofotometrede standart ve numunelerinin amlodipin besilatın metanoldeki çözeltilerinin 246 nm'deki valsartanın ise 234,3 ve 263 nm'lerdeki türev absorbans değerleri (dA/dλ) ölçülmüştür. Ölçülen bu değerlerde kalibrasyon grafiği çizme ve standart ekleme teknikleriyle etken madde miktar tayini yapılmıştır. Korelâsyon katsayıları, kalibrasyon grafiği çizme tekniğinde amlodipin besilat için 0,9992, valsartan için 0,9987 ve 0,9987; standart ekleme tekniğinde ise amlodipin besilat için 0,9987 ve valsartan için ise 0,9969 ve 0,9987 olarak hesaplanmıştır. Doğrudan UV ve birinci türev UV spektrofotometride doğrusal çalışma aralıkları amlodipin besilat için 3-18 mg/L, valsartan için ise 10-60 mg/L olarak hesaplanmıştır. Amlodipin besilat ve valsartan'ı birlikte içeren preparatlarda etken maddelerin aynı anda miktar tayinleri için iki yöntem önerilmiştir. Bu tezde ilk önerilen metot birinci türev UV spekktrofotometridir. Yöntemde standart ve numunelerin metanoldeki çözeltilerinin amlodipin besilat için 243,6 ve 248,8 nm'lerdeki ve valsartan için ise 237,2 ve 289 nm'lerdeki türev absorbans değerleri (dA/dλ) ölçülmüştür. Amlodipin besilat için 243,6 nm'de, valsartan için 289 nm'de kalibrasyon grafiği çizme ve standart ekleme teknikleriyle etken madde miktar tayini yapılmıştır. Yöntemde doğrusal çalışma aralıkları amlodipin besilat için 3–18 mg/L, valsartan için ise 10–60 mg/L olarak hesaplanmıştır. Korelâsyon katsayıları, kalibrasyon grafiği çizme tekniğinde amlodipin besilat için 0,9997 ve 0,9965, valsartan için 0,9992 ve 0,9979; standart ekleme tekniğinde ise amlodipin besilat için 0,9973 ve valsartan için ise 0,9973 olarak hesaplanmıştır. İkinci olarak önerilen yöntem spektrum oranları birinci türev spektrofotometridir. Yöntemde standart ve numunelerin metanoldeki çözeltilerinin amlodipin besilat için 334,4 nm'deki ve valsartan için ise 231,3 nm'deki türev absorbans değerleri (dA/dλ) ölçülmüştür. Ölçülen bu değerlerde kalibrasyon grafiği çizme ve standart ekleme teknikleriyle etken madde tayini yapılmıştır. Yöntemde doğrusal çalışma aralıkları amlodipin besilat için 3-18 mg/L, valsartan için ise 10-60 mg/L olarak hesaplanmıştır. Korelâsyon katsayıları, kalibrasyon grafiği çizme tekniğinde amlodipin besilat için 0,9986, valsartan için 0,9989; standart ekleme tekniğinde ise amlodipin besilat için 0,9969 ve valsartan için ise 0,9975 olarak hesaplanmıştır. Önerilen bu spektrofotometrik yöntemler amlodipin besilat, valsartan ve amlodipin besilat-valsartan içeren preparatlara başarıyla uygulanmıştır.
In this thesis, spectrofotometric methods for efficient materials quantitative determination are proposed for the preparations including amlodipine and valsartan alone and amlodipine besylate + valsartan combination. Direct UV spectrofotometry and first derivative UV spectrofotometry have been proposed for the preparation including amlodipine and valsartan alone. In the direct UV spectrophotometry absorbance values of standard and sample solutions in methanol were measured at 237,3 and 360 nm's for amlodipine besylate and 249 nm's for valsartan, respectively. Calibration graphics plooting and standard addition method were used to determine drug active compounds in measured values. The correlation coefficents were calculated as 0,9994 and 0,9990 for amlodipine besylat, 0,9997 for valsartan by calibration graphic plooting technique; 1,0000 and 0,9962 for amlodipine besylat and 0,9989 for valsartan by standard addition method. On the other method, first derivative UV spectrphotometry, solutions of standard and samples derivative absorbance (dA/dλ) signals were measured at 246 nm' amlodipine besylate and 237,3 and 263 nm' for valsartan, respectively. Calibration graphics plooting and standard addition method were used to determine drug active compounds in measured signals. The correlation coefficents were calculated as 0,9992 for amlodipine besylat, 0,9987 and 0,9987 for valsartan by calibration graphic plooting technique; 0,9987 for amlodipine besylat and 0,9969 and 0,9987 for valsartan by standard adding technique. Linear working range was established as 3,0 - 18,0 mg/L for amlodipine besylate and 10,0-60,0 mg/L for valsartan for both methods. Two methods are proposed for the simultaneous determination of the preparations containing amlodipine besiylat and valsartan combination. In this thes, the first proposed method is first derivative spectrofotometry. Solutions of standart and samples in methanol derivative absorbance (dA/dλ) values were measured at 243,6 and 248,8 nm' for amlodipine besylate and 237,2 and 289 nm's for valsartan, respectively. Calibration graphics plooting and standard addition method were used to determine drug active compounds at 243,6 nm's for amlodipine besylat and 289 nm's for valsartan. In this method, the calibration curve for amlodipine besylate and valsartan demonstrated linearity in the range 3,0 – 10,0 mg/L and 10,0 – 60 mg/L, respectively. The correlation coefficent were calculated as 0,9997 and 0,9965 for amlodipine besylat, 0,9992 and 0,9979 for valsartan by calibration graphic plooting technique; 0,9973 for amlodipine besylat and 0,9973 for valsartan by standard addition technique. The secondly proposed method in this thesis is ratio spectra first derivative spectrophotometry. Solituons of standart and samples in methanol ratio spectra derivative absorbance (dA/dλ) signals were measured at 344,4 nm for amlodipine besylate and 231,3 nm for valsartan, respectively. Calibration graphics plooting and standard addition method were used to determine drug active compounds in measured signals. In this method, the calibration curve for amlodipine besylat and valsartan demonstrated linearity in the range 3,0 – 10,0 mg/L and 10,0 – 60 mg/L, respectively. The coefficents of correlation were calculated as 0,9986 for amlodipine besylat, 0,9989 for valsartan by calibration graphic plooting technique; 0,9969 for amlodipine besylat and 0,9975 for valsartan by standard addition method.
In this thesis, spectrofotometric methods for efficient materials quantitative determination are proposed for the preparations including amlodipine and valsartan alone and amlodipine besylate + valsartan combination. Direct UV spectrofotometry and first derivative UV spectrofotometry have been proposed for the preparation including amlodipine and valsartan alone. In the direct UV spectrophotometry absorbance values of standard and sample solutions in methanol were measured at 237,3 and 360 nm's for amlodipine besylate and 249 nm's for valsartan, respectively. Calibration graphics plooting and standard addition method were used to determine drug active compounds in measured values. The correlation coefficents were calculated as 0,9994 and 0,9990 for amlodipine besylat, 0,9997 for valsartan by calibration graphic plooting technique; 1,0000 and 0,9962 for amlodipine besylat and 0,9989 for valsartan by standard addition method. On the other method, first derivative UV spectrphotometry, solutions of standard and samples derivative absorbance (dA/dλ) signals were measured at 246 nm' amlodipine besylate and 237,3 and 263 nm' for valsartan, respectively. Calibration graphics plooting and standard addition method were used to determine drug active compounds in measured signals. The correlation coefficents were calculated as 0,9992 for amlodipine besylat, 0,9987 and 0,9987 for valsartan by calibration graphic plooting technique; 0,9987 for amlodipine besylat and 0,9969 and 0,9987 for valsartan by standard adding technique. Linear working range was established as 3,0 - 18,0 mg/L for amlodipine besylate and 10,0-60,0 mg/L for valsartan for both methods. Two methods are proposed for the simultaneous determination of the preparations containing amlodipine besiylat and valsartan combination. In this thes, the first proposed method is first derivative spectrofotometry. Solutions of standart and samples in methanol derivative absorbance (dA/dλ) values were measured at 243,6 and 248,8 nm' for amlodipine besylate and 237,2 and 289 nm's for valsartan, respectively. Calibration graphics plooting and standard addition method were used to determine drug active compounds at 243,6 nm's for amlodipine besylat and 289 nm's for valsartan. In this method, the calibration curve for amlodipine besylate and valsartan demonstrated linearity in the range 3,0 – 10,0 mg/L and 10,0 – 60 mg/L, respectively. The correlation coefficent were calculated as 0,9997 and 0,9965 for amlodipine besylat, 0,9992 and 0,9979 for valsartan by calibration graphic plooting technique; 0,9973 for amlodipine besylat and 0,9973 for valsartan by standard addition technique. The secondly proposed method in this thesis is ratio spectra first derivative spectrophotometry. Solituons of standart and samples in methanol ratio spectra derivative absorbance (dA/dλ) signals were measured at 344,4 nm for amlodipine besylate and 231,3 nm for valsartan, respectively. Calibration graphics plooting and standard addition method were used to determine drug active compounds in measured signals. In this method, the calibration curve for amlodipine besylat and valsartan demonstrated linearity in the range 3,0 – 10,0 mg/L and 10,0 – 60 mg/L, respectively. The coefficents of correlation were calculated as 0,9986 for amlodipine besylat, 0,9989 for valsartan by calibration graphic plooting technique; 0,9969 for amlodipine besylat and 0,9975 for valsartan by standard addition method.
Açıklama
Anahtar Kelimeler
Amlodipin besilat, Amlodipine besylate, Valsartan birinci türev spektrofotometri, First derivative spectrophotometry, Doğrudan UV spektrofotometri;, Direct UV spectrophotometry, Korelasyon katsayısı, Standart adding, Spektrum oranları birinci türev spektrofotometri, Spectrum ratio first derivative spectrophotometry
Kaynak
WoS Q Değeri
Scopus Q Değeri
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Sayı
Künye
Uysal, H. (2014). Bazı ilaç etken maddelerin tayini için türev spektrofotometrik yöntem geliştirilmesi. Selçuk Üniversitesi, Yayımlanmış yüksek lisans tezi, Konya.
