İbuprofenin Farmasötik Preperatlarda UPLC-MS/MS Yöntemiyle Tayini

Year 2022, , 58 - 63, 29.06.2022

Ömer Faruk Koçak , Alptuğ Atila

https://doi.org/10.46810/tdfd.1107889

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

References

• [1] Hong S, Xu K, Guo S, Yuan L, Wang H. Development and Validation of a New Simple HPLC Method for the Determination of 3-[4-(2-Methylpropyl)phenyl] Propanoic Acid as an Impurity of Ibuprofen and Ibuprofen Sodium. Chromatographia. 2017 Jul 1;80(7):1095–100.
• [2] Ragab MAA, Abdel-Hay MH, Ahmed HM, Mohyeldin SM. Determination of ibuprofen and phenylephrine in tablets by high-performance thin layer chromatography and in plasma by high-performance liquid chromatography with diode array detection. J Chromatogr Sci. 2019;57(7):1–8.
• [3] Puangpetch A, Limrungsikul A, Prommas S, Rukthong P, Sukasem C. Development and validation of a liquid chromatography-tandem mass spectrometry method for determination of ibuprofen in human plasma. Clin Mass Spectrom [Internet]. 2020;15:6–12. Available from: https://doi.org/10.1016/j.clinms.2019.10.002
• [4] Konstan MW, Byard PJ, Hoppel CL, Davis PB. Effect of High-Dose Ibuprofen in Patients with Cystic Fibrosis. N Engl J Med. 1995 Mar 30;332(13):848–54.
• [5] Asif U, Sherwani AK, Akhtar N, Shoaib MH, Hanif M, Qadir MI, et al. Formulation Development and Optimization of Febuxostat Tablets by Direct Compression Method. Adv Polym Technol. 2016;35(2).
• [6] Waraksa E, Wójtowicz-Zawadka M, Kwiatkowska D, Jarek A, Małkowska A, Wrzesień R, et al. Simultaneous determination of ibuprofen and its metabolites in complex equine urine matrices by GC-EI-MS in excretion study in view of doping control. J Pharm Biomed Anal. 2018;152:279–88.
• [7] Padró JM, Osorio-Grisales J, Arancibia JA, Olivieri AC, Castells CB. Enantiomeric analysis of overlapped chromatographic profiles in the presence of interferences. Determination of ibuprofen in a pharmaceutical formulation containing homatropine. J Chromatogr A [Internet]. 2016;1467:255–60. Available from: http://dx.doi.org/10.1016/j.chroma.2016.05.094
• [8] Ubale M, 1P.G.Dept. of Chemistry, Vasantrao Naik Mahavidyalaya A. RP-HPLC Method for Simultaneous Determination of Amlodipine Besylate and Atorvastatin Calcium : Application to Commerciallyavailable drug products. Int Arch App Sci Technol. 2014;5(1):22–7.
• [9] Ali NW, Hegazy MA, Abdelkawy M, Abdelaleem EA. Simultaneous determination of methocarbamol and its related substance (guaifenesin) in two ternary mixtures with ibuprofen and diclofenac potassium by RP-HPLC method. J Liq Chromatogr Relat Technol. 2012;35(16):2229–42.
• [10] Cunha RR, Chaves SC, Ribeiro MMAC, Torres LMFC, Muñoz RAA, Santos WTPD, et al. Simultaneous determination of caffeine, paracetamol, and ibuprofen in pharmaceutical formulations by high-performance liquid chromatography with UV detection and by capillary electrophoresis with conductivity detection. J Sep Sci. 2015;38(10):1657–62.
• [11] Shah DA, Suthar DJ, Nagda CD, Chhalotiya UK, Bhatt KK. Development and validation of hptlc method for estimation of ibuprofen and famotidine in pharmaceutical dosage form. J Liq Chromatogr Relat Technol. 2014;37(7):941–50.
• [12] Ragab MAA, Korany MA, Michail K, Issa AE, Daabees HM, Elkafrawy DS. Discrete fourier transform convoluted densitomteric peak responses for the determination of methocarbamol in different pharmaceutical mixtures in the presence of its degradation product. J Liq Chromatogr Relat Technol. 2014;37(14):1999–2020.
• [13] El-Kimary EI, Ragab MAA. Derivative synchronous spectrofluorimetry: Application to the analysis of two binary mixtures containing codeine in dosage forms. Spectrochim Acta - Part A Mol Biomol Spectrosc [Internet]. 2018;204:677–84. Available from: https://doi.org/10.1016/j.saa.2018.06.102
• [14] Damiani PC, Bearzotti M, Cabezón MA. Spectrofluorometric determination of ibuprofen in pharmaceutical formulations. J Pharm Biomed Anal. 2001;25(3–4):679–83.
• [15] Nováková L, Matysová L, Solich P. Advantages of application of UPLC in pharmaceutical analysis. Talanta. 2006;68(3):908–18.
• [16] Gumustas M, Kurbanoglu S, Uslu B, Ozkan SA. UPLC versus HPLC on drug analysis: Advantageous, applications and their validation parameters. Vol. 76, Chromatographia. 2013. 1365–1427 p.
• [17] Kumar A, Saini G, Nair A, Sharma R. A preeminent technique in pharmaceutical analysis. Acta Pol Pharm. 2012;69(3):371–80.
• [18] Mensch J, Noppe M, Adriaensen J, Melis A, Mackie C, Augustijns P, et al. Novel generic UPLC/MS/MS method for high throughput analysis applied to permeability assessment in early Drug Discovery. J Chromatogr B Anal Technol Biomed Life Sci. 2007;847(2):182–7.
• [19] Yaman ME, Atila A. A rapid and sensitive UPLC – MS / MS method for quantification of erdosteine as bulk drug and in capsules as dosage forms. Maced Pharm Bull. 2021;67(2):23–31.
• [20] Borman P, guidelines DE-IQ, 2017 undefined. Q2 (R1) validation of analytical procedures. books.google.com [Internet]. [cited 2022 Apr 23]; Available from: https://www.google.com/books?hl=tr&lr=&id=Wvk1DwAAQBAJ&oi=fnd&pg=PA127&dq=Borman,+P.,+Elder,+D.,+2017.+Validation+of+analytical+procedures:+text+and+methodology.+Q2+(R1).++++++++++++++ICH+Quality+guidelines+5,+127-166.++&ots=pM8d8-hhC3&sig=p5XLtMsyb19nwZk69Gh6Xb0FQOU
• [21] Method Validation in Pharmaceutical Analysis: A Guide to Best Practice - Google Kitaplar [Internet]. [cited 2022 Apr 23]. Available from: https://books.google.com.tr/books?hl=tr&lr=&id=HbBlyvlRgwkC&oi=fnd&pg=PR5&dq=Ermer,+J.,+Miller,+J.H.M.,+2006.+Method+validation+in+pharmaceutical+analysis:+A+guide+to+best+practice,+first+ed.+John+Wiley+%26+Sons.&ots=nWFpDMC5Oi&sig=1SoZdUvr6p2UBIFTI5z-IirtZBg&redir_esc=y#v=onepage&q&f=false
• [22] (R1) IG-Q, 2005 undefined. Validation of analytical procedures: text and methodology. somatek.com [Internet]. 2014 [cited 2022 Apr 23]; Available from: https://somatek.com/wp-content/uploads/2014/06/sk140605h.pdf
• [23] Sherwood CA, Eastham A, Lee LW, Risler J, Mirzaei H, Falkner JA, et al. Rapid optimization of MRM-MS instrument parameters by subtle alteration of precursor and product m/z targets. J Proteome Res. 2009;8(7):3746–51.
• [24] Battu PR, MS Reddy. RP-HPLC Method for Simultaneous Estimation of Paracetamol and Ibuprofen in Tablets. Asian J Res Chem. 2009;2(1):70–2.
• [25] Eraga SO, Arhewoh MI, Chibuogwu RN, Iwuagwu MA. A comparative UV−HPLC analysis of ten brands of ibuprofen tablets. Asian Pac J Trop Biomed [Internet]. 2015 Oct;5(10):880–4. Available from: http://linkinghub.elsevier.com/retrieve/pii/S2221169115001379
• [26] Borahan T, Unutkan T, Şahin A, Bakırdere S. A rapid and sensitive reversed phase-HPLC method for simultaneous determination of ibuprofen and paracetamol in drug samples and their behaviors in simulated gastric conditions. J Sep Sci [Internet]. 2019 Feb;42(3):678–83. Available from: http://dx.doi.org/10.1016/j.apjtb.2015.06.005
• [27] Sanchaniya PM, Mehta FA, Uchadadiya NB. Development and Validation of an RP-HPLC Method for Estimation of Chlorpheniramine Maleate, Ibuprofen, and Phenylephrine Hydrochloride in Combined Pharmaceutical Dosage Form. Chromatogr Res Int. 2013;2013:1–6.
• [28] Arayne MS, Sultana N, Siddiqui FA, Naseem S, Qureshi F. Simultaneous determination of pyrimethamine, sulfadoxine, mefloquine, and ibuprofen in pharmaceutical formulations by RP-HPLC. Med Chem Res. 2010;19(9):1043–54.