Determination of Ibuprofen using Derivatization with MSTFA in Pharmaceutical Preparations by GC-MS Method

Abstract

Objective: The aim of this study was to develop and validate a gas chromatography-mass spectrometry (GC-MS) method for the analysis of ibuprofen in both its pure form and pharmaceutical formulations. Methods: A GC-MS method was developed and validated to determine the concentration of ibuprofen. The method's linearity was assessed over a concentration range of 0.5-10 µg mL-1. The intra- and inter-day precision was evaluated, with relative standard deviations calculated. Detection and quantification limits were determined. Stability tests were conducted to assess the stability of ibuprofen solutions at different temperatures. The potential interference of tablet excipients was also evaluated. Results: The GC-MS method demonstrated linearity in the range of 0.5-10 µg mL-1. The intra- and inter-day relative standard deviations were below 1.17% and 3.71%, respectively. The detection limit was 0.15 µg mL-1, and the quantification limit was 0.45 µg mL-1. Stability tests showed that ibuprofen remained stable in solution for 24 hours at room temperature, and up to 72 hours when stored at both 4 °C and -20 °C. No interference from tablet excipients was observed. Conclusion: The GC-MS method is effective for quantifying ibuprofen in both pure form and pharmaceutical formulations. The method provides reliable results with good precision, stability, and no interference from excipients, making it suitable for ensuring the consistency of formulation content in commercial ibuprofen dosage forms.

Keywords

• Ibuprofen
• GC-MS
• Validation
• Tablet

GC-MS Yöntemi ile İbuprofenin Farmasötik Preparatlarda MSTFA ile Derivatizasyon Kullanılarak Belirlenmesi

Öz

Amaç: Bu çalışmanın amacı, ibuprofenin saf formu ve farmasötik formülasyonlarında analiz edilmesi için bir gaz kromatografisi-kütle spektrometrisi (GC-MS) yöntemini geliştirmek ve doğrulamaktır. Yöntemler: İbuprofen konsantrasyonunu belirlemek için bir GC-MS yöntemi geliştirilmiş ve doğrulanmıştır. Yöntemin doğrusalığı, 0.05-5.0 µg mL-1 arasındaki konsantrasyon aralığında değerlendirilmiştir. İntra ve inter-gün hassasiyetleri, yüzde göreli standart sapmalar hesaplanarak değerlendirilmiştir. Tespit ve nicem sınırları belirlenmiştir. İbuprofen çözeltilerinin farklı sıcaklıklarda stabilitesini değerlendirmek için stabilite testleri yapılmıştır. Ayrıca, tablet eksipiyanlarının potansiyel interferansı da değerlendirilmiştir. Bulgular: GC-MS yöntemi, 0.05-5.0 µg mL-1 aralığında doğrusal bir ilişki göstermiştir. İntra ve inter-gün yüzde göreli standart sapmalar sırasıyla %1.18'in ve %3.51'in altında bulunmuştur. Tespit sınırı 0.015 µg mL-1 ve nicem sınırı 0.045 µg mL-1 olarak belirlenmiştir. Stabilite testleri, ibuprofenin oda sıcaklığında 24 saat, 4 °C ve -20 °C’de ise 72 saate kadar stabil kaldığını göstermiştir. Tablet eksipiyanlarından herhangi bir interferans gözlemlenmemiştir. Sonuç: GC-MS yöntemi, ibuprofenin saf formu ve farmasötik formülasyonlarında kantifikasyonu için etkilidir. Yöntem, iyi bir doğruluk, stabilite ve eksipiyanlardan hiçbir interferans olmadan güvenilir sonuçlar sağlamakta olup, ticari ibuprofen dozaj formlarında formülasyon içeriğinin tutarlılığını sağlamak için uygun bir yöntemdir.

Anahtar Kelimeler

• Ibuprofen
• GC-MS
• Validation
• Tablet

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