FARMASÖTİK DOZAJ FORMUNDAN KAPTOPRİL TAYİNİ İÇİN YENİ STABİLİTE- GÖSTERGELİ RP-HPLC YÖNTEMİNİN YEŞİL PROSEDÜR İNDEKSİ DEĞERLENDİRİLMESİ

Year 2023, Volume: 47 Issue: 3, 894 - 906, 20.09.2023

Cem Erkmen , Bengi Uslu

https://doi.org/10.33483/jfpau.1319958

Cited By: 1

Abstract

Amaç: Bu çalışmada, yaygın bir ağrı kesici olan parasetamol iç standart olarak kullanarak antihipertansif ilaç kaptopril’in ultra-hassas tayini için yeni bir ters fazlı sıvı kromatografi yönteminin geliştirilmesi amaçlanmıştır. Mobil faz bileşimi, akış hızı, kolon sıcaklığı gibi tüm deneysel koşulların optimizasyonu adım adım gerçekleştirilmiş ve geliştirilen yöntemin yöntem geçerliliği uluslararası validasyon kılavuzlarına göre incelenmiştir. Kalibrasyon aralığı, doğrusallık, tespit limiti, tayin limiti, sağlamlık, ticari tablet numunelerinden doğruluk ve metot stabilitesi detaylı olarak incelenmiştir. Ayrıca geliştirilen yöntemin yeşillik profili, literatürde sıklıkla kullanılan Yeşil Analitik Prosedür İndeksi ve Analitik Yeşillik Hesaplayıcı teknikleri ile değerlendirilmiştir.
Gereç ve Yöntem: Kromatografik yöntem, tamamen gözenekli silika materyaller ile doldurulmuş bir XBridge C18 kolonu (25 cm x 4.6 mm ID; 5 µm) ile gerçekleştirildi. Tüm analizler, 1.5 ml dk-1 akış hızında asetonitril:5 mM, pH 7.0 amonyum asetat çözeltisi (50:50, v/v) içeren bir mobil faz ile izokratik olarak yapıldı. Enjeksiyon hacmi 5 µl idi ve kolon, bir kolon fırınında 25°C’de sabit tutuldu. Kolon eluatı 220 nm’de izlendi. Optimize edilmiş koşullar altında, kaptopril ve parasetamolün alıkonma süreleri sırasıyla yaklaşık 1.59 ve 2.0 dakika olmuştur.
Sonuç ve Tartışma: Bu çalışma, tablet numunelerinde kaptopril tayini için tam olarak doğrulanmış, basit, hassas, doğru, doğrusal, kesin ve tekrar üretilebilir bir ters fazlı sıvı kromatografi yöntemini tanımlamıştır. Optimal deneysel koşullar altında lineer aralık 0.5-200 µg ml-1 aralığında bulundu ve korelasyon katsayısı 0,99'dan büyüktü. Yöntem kesinliği, %0.05 ile %0.61 arasındaki varyasyon katsayıları ile kabul edilebilir düzeydeydi. Ayrıca tablet numuneleri üzerinde yapılan geri kazanım çalışmaları sonucunda doğruluğun %99.45 ile %102.55 arasında tatmin edici sınırlar içinde olduğu görülmüştür. Ayrıca geliştirilen yöntemin yeşillik profili de yöntemin çevre dostu olduğunu göstermiştir.

Keywords

Analitik yeşillik değerlendirmesi, HPLC, kaptopril, optimizasyon, validasyon

GREEN PROCEDURE INDEX ASSESSMENT OF THE NOVEL STABILITY-INDICATING RP-HPLC METHOD FOR THE DETERMINATION OF CAPTOPRIL FROM PHARMACEUTICAL DOSAGE FORM

Abstract

Objective: In this study, it was aimed to develop a novel reverse-phase liquid chromatography method for the ultra-sensitive determination of the antihypertensive drug captopril, using paracetamol, which is the common pain killer, as the internal standard. Optimization of all experimental conditions including composition of mobile phase, flow rate, and column temperature was carried out step by step, and the method validity of the developed method was examined according to international validation guidelines. Calibration range, linearity, the limit of determination, the limit of quantification, robustness, accuracy from commercial tablet samples, and method stability were examined in detail. In addition, the greenness profile for the developed method was assessed with the Green Analytical Procedure Index and Analytical Greenness Calculator techniques, which are frequently used in the literature.
Material and Method: The chromatographic method was conducted with an XBridge C18 column (25 cm x 4.6 mm ID; 5 µm) packed with fully porous silica materials. All analyses were performed isocratically with a mobile phase containing acetonitrile:5 mM, pH 7.0 ammonium acetate solution (50:50, v/v) at a flow rate of 1.5 ml min-1. The injection volume was 5 μl, and the column was kept at 25°C in a column oven. The column eluate was monitored at 220 nm. Under optimized conditions, retention times of captopril, and paracetamol were approximately 1.59, and 2.0 min, respectively.
Result and Discussion: This study described a fully validated, simple, sensitive, accurate, linear, precise, and reproducible reversed-phase liquid chromatography method for the determination of captopril in tablet samples. Under optimal experimental conditions, the linear range was found in the range of 0.5-200 µg ml-1 and the correlation coefficient was greater than 0.99. Method precision was acceptable, with coefficients of variation between 0.05% and 0.61%. In addition, as a result of the recovery studies carried out on the tablet samples, the accuracy was found to be within satisfactory limits between 99.45% and 102.55%. Moreover, the greenness profile of the developed method also showed that the method is environmentally friendly.

Keywords

Analytical greenness assessment, captopril, HPLC, optimization, validation

References

• 1. Saxena, M., Antoniou, S., Hamedi, N., Robinson, P., Singh, H., Mukhtar, O., Kapil, V., Lobo, M.D. (2016). Multiple drug-intolerant hypertension: A case series utilising a novel-treatment algorithm. British Journal of General Practice, 66(645), e285-e287. [CrossRef]
• 2. Jadam, M.L., Jubri, Z., Sarijo, S.H. (2023). Release behavior and cytotoxicity of captopril-intercalated layered double hydroxide for an antihypertensive drug delivery system. Journal of Porous Materials, 30(1), 223-233. [CrossRef]
• 3. Amar, M., Lam, S.W., Faulkenberg, K., Perez, A., Tang, W.W., Williams, J.B. (2021). Captopril versus hydralazine-isosorbide dinitrate vasodilator protocols in patients with acute decompensated heart failure transitioning from sodium nitroprusside. Journal of Cardiac Failure, 27(10), 1053-1060. [CrossRef]
• 4. Tandeter, H. (2016). Hypothesis: A single dose of an anxiolitic may prevent unnecessary visits to the emergency room during blood pressure elevations. Medical Hypotheses, 88, 35-37. [CrossRef]
• 5. Coulter, D.M., Edwards, I.R. (1987). Cough associated with captopril and enalapril. British Medical Journal (Clinical Research Ed.), 294(6586), 1521-1523. [CrossRef]
• 6. Ward, A., Brogden, R.N., Heel, R.C., Speight, T.M., Avery, G.S. (1983). Amrinone: A preliminary review of its pharmacological properties and therapeutic use. Drugs, 26, 468-502. [CrossRef]
• 7. Suarez, W.T., Madi, A.A., Figueiredo-Filho, L., Fatibello-Filho, O. (2007). Flow-injection spectrophotometric system for captopril determination in pharmaceuticals. Journal of the Brazilian Chemical Society, 18, 1215-1219. [CrossRef]
• 8. Mazurek, S., Szostak, R. (2006). Quantitative determination of captopril and prednisolone in tablets by FT-Raman spectroscopy. Journal of Pharmaceutical and Biomedical Analysis, 40(5), 1225-1230. [CrossRef]
• 9. Hillaert, S., Van den Bossche, W. (1999). Determination of captopril and its degradation products by capillary electrophoresis. Journal of Pharmaceutical and Biomedical Analysis, 21(1), 65-73. [CrossRef]
• 10. Karimi-Maleh, H., Ganjali, M.R., Norouzi, P., Bananezhad, A. (2017). Amplified nanostructure electrochemical sensor for simultaneous determination of captopril, acetaminophen, tyrosine and hydrochlorothiazide. Materials Science and Engineering: C, 73, 472-477. [CrossRef]
• 11. Beitollahi, H., Taher, M.A., Ahmadipour, M., Hosseinzadeh, R. (2014). Electrocatalytic determination of captopril using a modified carbon nanotube paste electrode: Application to determination of captopril in pharmaceutical and biological samples. Measurement, 47, 770-776. [CrossRef]
• 12. Khalilzadeh, M.A., Karimi-Maleh, H., Amiri, A., Gholami, F. (2010). Determination of captopril in patient human urine using ferrocenemonocarboxylic acid modified carbon nanotubes paste electrode. Chinese Chemical Letters, 21(12), 1467-1470. [CrossRef]
• 13. Rezaei, B., Damiri, S. (2008). Voltammetric behavior of multi-walled carbon nanotubes modified electrode-hexacyanoferrate (II) electrocatalyst system as a sensor for determination of captopril. Sensors and Actuators B: Chemical, 134(1), 324-331. [CrossRef]
• 14. Muhire, J., Li, B.Q., Zhai, H.L., Wang, X., Xu, M.L. (2019). A fast chemometrics approach to quantitative analysis of metformin hydrochloride, enalapril maleate, and captopril in tablets based on HPLC-PAD spectra. Acta Chromatographica, 31(3), 228-234. [CrossRef]
• 15. Gatti, R., Morigi, R. (2017). 1,4-Anthraquinone: A new useful pre-column reagent for the determination of N-acetylcysteine and captopril in pharmaceuticals by high performance liquid chromatography. Journal of Pharmaceutical and Biomedical Analysis, 143, 299-304. [CrossRef]
• 16. Rastkari, N., Khoobi, M., Shafiee, A., Khoshayand, M.R., Ahmadkhaniha, R. (2013). Development and validation of a simple and sensitive HPLC-UV method for the determination of captopril in human plasma using a new derivatizing reagent 2-naphthyl propiolate. Journal of Chromatography B, 932, 144-151. [CrossRef]
• 17. Dawud, E.R., Shakya, A.K. (2019). HPLC-PDA analysis of ACE-inhibitors, hydrochlorothiazide and indapamide utilizing design of experiments. Arabian Journal of Chemistry, 12(5), 718-728. [CrossRef]
• 18. Carje, A.G., Balint, A., Ion, V., Pop, A.L., Muntean, D.L., Sabau, R., Imre, S. (2019). HPLC-UV method approach for the analysis and impurity profiling of captopril. Studia Universitatis. Babes-Bolyai Chemia, 64(2T1), 231-242. [CrossRef]
• 19. ICH Q1A (R2). (2003). International Conference on Harmonization (ICH). Guidance for Industry: Q1A (R2) Stability Testing of new Drug Substances and Products. Ich Harmonised Tripartite Guideline, 4. from https://www.ema.europa.eu/en/documents/scientific-guideline/ich-q-1-r2-stability-testing-new-drug-substances-products-step-5_en.pdf. Accessed date: 17.01.2023.
• 20. Harron, D.W. (2013). Technical requirements for registration of pharmaceuticals for human use: The ICH process. The Textbook of Pharmaceutical Medicine, 447-460. [CrossRef]
• 21. Guideline, I.H.T. (2022). Validation of analytical procedures: Text and methodology Q2 (R1). ICH: Geneva, Switzerland. From https://database.ich.org/sites/default/files/Q2%28R1%29%20Guideline.pdf. Accessed date: 20.01.2023.
• 22. Arayne, M.S., Sultana, N., Zuberi, M.H., Siddiqui, F.A., Haroon, U. (2013). Simultaneous determination of metformin, captopril, lisinopril, and enalapril by RP-HPLC: its applications in dosage formulations and in human serum. Medicinal Chemistry Research, 22, 5717-5722. [CrossRef]
• 23. Shafi, N., Siddiqui, F.A., Sultana, N., Arayne, M.S. (2015). Concurrent determination of diltiazem, lisinopril, captopril, and enalapril in dosage formulations and in human serum by liquid chromatographic technique. Journal of Liquid Chromatography & Related Technologies, 38(15), 1466-1473. [CrossRef]
• 24. Sultana, N., Arayne, M.S., Ali, S.N. (2013). Liquid chromatographic method for the simultaneous determination of captopril, piroxicam, and amlodipine in bulk drug, pharmaceutical formulation, and human serum by programming the detector. Journal of Separation Science, 36(19), 3176-3183. [CrossRef]
• 25. El-Gindy, A., Nassar, M.W., Attia, K.A.S., Abu-Seada, H.H., El-Ghandour, M. (2014). Stability-Indicating HPLC method for simultaneous determination of captopril, indapamide, and their related compounds. Journal of Liquid Chromatography & Related Technologies, 37(5), 696-712. [CrossRef]
• 26. El-Maraghy, C.M. (2023). Implementation of green chemistry to develop HPLC/UV and HPTLC methods for the quality control of Fluconazole in presence of two official impurities in drug substance and pharmaceutical formulations. Sustainable Chemistry and Pharmacy, 33, 101124. [CrossRef]
• 27. Sajid, M., Płotka-Wasylka, J. (2022). Green analytical chemistry metrics: A review. Talanta, 238, 123046. [CrossRef]
• 28. Płotka-Wasylka, J. (2018). A new tool for the evaluation of the analytical procedure: Green Analytical Procedure Index. Talanta, 181, 204-209. [CrossRef]
• 29. Bahgat, E.A., Saleh, H., Reda, A., Fawzy, M.G. (2022). Development and validation of eco-friendly micellar organic solvent-free HPLC method for the simultaneous determination of some antihypertensive combinations. Microchemical Journal, 181, 107740. [CrossRef]
• 30. Huang, T., He, Z., Yang, B., Shao, L., Zheng, X., Duan, G. (2006). Simultaneous determination of captopril and hydrochlorothiazide in human plasma by reverse-phase HPLC from linear gradient elution. Journal of Pharmaceutical and Biomedical Analysis, 41(2), 644-648. [CrossRef]