İbuprofenin Farmasötik Preperatlarda UPLC-MS/MS Yöntemiyle Tayini

Abstract

İbuprofen (IBU), yaygın olarak reçete edilen, steroid olmayan bir anti-inflamatuar ilaçtır. Farmasötik formülasyonlarda IBU'nun belirlenmesi için tandem üçlü dörtlü kütle spektrometrisi ile kombinasyon halinde hassas, basit, doğru ve hızlı ultra performanslı sıvı kromatografi yöntemi (UPLC-MS/MS) yöntemi kullanılmış ve doğrulanmıştır. Kromatografik ayırma, bir C18 UPLC kolonu, 95 Å, 2.1 x 50 mm, 1.8 µm ve asetonitril ile birlikte yüzde 0.1’lik formik asit (25:75 v/v) kullanılarak gerçekleştirildi. Akış hızı, 2.0 dakikalık bir çalışma süresi ile 0.15 ml dak-1 idi. Enjeksiyon hacmi 5 μL ve kolon sıcaklığı 40 °C'de sabit tutuldu. İbuprofen ve IS kütle geçişleri sırasıyla m/z 205.1 → 159.0 ve 249.9 → 229.1 idi. ICH yönergelerine göre, yaklaşım tamamen doğrulandı. 1-5000 ng mL-1 kalibrasyon eğrisi doğrusal aralığı, güçlü bir korelasyon katsayısına (0.9921) sahipti. Gün içi ve günler arası kesinlik, bağıl standart sapma olarak ifade edildi ve %6.24'ten düşüktü. Bu yöntem, hem saf formda hem de farmasötik formülasyonlarda IBU'yu büyük bir başarıyla belirlemek için kullanılmıştır.

Keywords

• İbuprofen
• UPLC-MS/MS
• Farmasötik analiz

Determination of Ibuprofen in Pharmaceutical Preparations by UPLC-MS/MS Method

Abstract

Ibuprofen (IBU) is a non-steroidal anti-inflammatory drug that is extensively prescribed. For the determination of IBU in pharmaceutical formulations, a sensitive, simple, accurate, and rapid ultra-performance liquid chromatography method in combination with tandem triple quadruple mass spectrometry (UPLC-MS/MS) has been used and validated. The chromatographic separation was accomplished using a C18 UPLC column, 95 Å, 2.1 x 50 mm, 1.8 µm, and 0.1 percent formic acid in conjunction with acetonitrile (25:75 v/v. The flow rate was 0.15 ml min-1, with a run duration of 2.0 minutes. The injection volume was 5 μL and the column temperature was held constant at 40 °C.The mass transitions of İbuprofen and IS were m/z 205.1 → 159.0 and 249.9 → 229.1, respectivelty. According to ICH guidelines, the approach was thoroughly verified. The linear range 1-5000 ng mL-1 calibration curve has a strong correlation coefficient (0.9921). Within and between days precision were expressed as relative standard deviation and were lower than 6.24%. This method has been used to determine IBU in both pure form and pharmaceutical formulations with great success.

Keywords

• Ibuprofen
• UPLC-MS/MS
• Pharmaceutical analysis

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