Araştırma Makalesi
BibTex RIS Kaynak Göster

Analytical QbD based systematic development of a novel RP-UHPLC method for the quantification of albuterol sulphate in its metered dose inhaler formulations

Yıl 2021, Cilt: 25 Sayı: 5, 689 - 701, 28.06.2025

Bikash Ranjan Jena Siva Prasad Panda Umasankar Kulandaivelu Rajasekhar Reddy Alavala G.s.n. Koteswara Rao Debashish Ghose Gurudutta Pattnaik Debi Prasad Pradhan

Öz

Albuterol sulphate is a Beta-2–adrenergic agonist drug mainly used in the form of nasal inhalations to treat chronic bronchitis and chronic obstructive pulmonary disease (COPD). A simple, rapid, precise chemometrics- based RP-UHPLC method has been developed and validated in its MDI formulations by the QbD approach. The chromatographic separation was achieved by Hibar HR purospher STAR RP-18 encapped column (C18, 250 mm × 4.6 mm, 5 μm) with UV detection λmax 225 nm. The retention time (Rt) for albuterol sulphate was observed as 2.434 over a run time of 5 minutes. Optimization of the method for the quantification of albuterol sulphate in its metered dose inhaler formulations has been performed by using 22 central composite design with response surface methodology that might lessen the solvent consumption, duration, and additional resources. A total of two independent variables, organic phase composition, and flow rate, were analyzed to construct a quadratic process model to examine the effect of independent variables or critical material attributes (CMAs) ahead the observed responses known as the critical method parameters (CMPs) within the designed space. The optimized UHPLC method contains phosphate buffer (10 mM KH2PO4) and acetonitrile (60:40 %v/v) as the mobile phase, which was delivered with a flow rate of 1.0 ml/min and the column was maintained at 40°C. The developed QbD based method was subsequently validated as per ICH Q2 R1 guidelines. The method obeyed linearity within the range of (5-120 μg/mL) with regression R2 of 0.999 for albuterol sulphate. The low coefficients of variation obtained in the intraday and inter-day precision studies indicate précised method. High recovery of albuterol sulphate has been observed within the range of (98.0-102.0 %). The developed method can be intensely employed as a highly robust, accurate, and cost-effective for routine analysis in research labs that competitively separate the drug from its excipients.

Anahtar Kelimeler

Accuracy validation isocratic experimental design albuterol sulphate correlation coefficient

Kaynakça

  • [1] Abdine HH, Belal F, Al-Badr AA. Ipratropium Bromide: Physical Properties. Prof of Drug Subs Exc and Rel Methodol. 2003; 30: 59-83.
  • [2] Kasawar BG, Farooqui M. Development and Validation of a Stability Indicating RP-HPLC Method for the Simultaneous Determination of Related Substances of Albuterol Sulphate and Ipratropium Bromide in Nasal Solution. J Pharm Biomed Anal. 2010; 52: 19–29.
  • [3] Sowjanya G, Gowri SD, & Rao JVLNS. Development and validation of a new RPHPLC method for the simultaneous determination of albuterol sulphate and ipratropium bromide in nasal inhalations. Int Res J Pharm. 2018; 9:63-70.
  • [4] Orlandini S, Pinzauti S, & Furlanetto S. Application of quality by design to the development of analytical separation methods. Anal Bioanal Chem. 2013; 405: 443-450.
  • [5] Debrus D, Guillarme S.R. Improved quality-by-design compliant methodology for method development in reversed- phase liquid chromatography. J Pharm Biomed Anal. 2013; 84: 215-223.
  • [6] Ramalingam P, Kalva B, Yiragamreddy PR. Analytical Quality by Design: A Tool for Regulatory Flexibility and Robust Analytics. Int J Anal Chem. 2015; 10: 1-9.
  • [7] Swain S, Jena BR, Madugula D, and Beg S. Application of Quality by Design Paradigms for Development of Solid Dosage Forms. In: Beg S, Hasnain MS. (Eds). Pharmaceutical Quality by Design. Academic Press, 2019. pp.109-130.
  • [8] Li Y, Terfloth, GJ, Kord AS. A systematic approach to RP-HPLC method development in a pharmaceutical QbD environment. Ame Pharm Rev. 2009; 12: 01-09.
  • [9] Swain S, Parhi R, Jena BR, Babu SM. Quality by Design: Concept to Applications. Curr Drug Discov Technol. 2019; 16: 1-11.
  • [10] Sahu PK, Ramisetti NR, Swain S Patro CS, Panda J. An overview of experimental designs in HPLC method development and validation. J Pharm Biomed Anal. 2018; 147: 590-611.
  • [11] Jena BR, Panda SP, Umasankar K, Swain S, X Rao GSNK, Damayanthi D, Ghose D, Pradhan DP. Applications of QbD-based Software in Analytical Research and Development. Curr Pharm Anal. 2021; (17)1: 461-473.
  • [12] Allen TT, Design of Experiments and Other Six Sigma Related Methods Explained and Derived, Thomson Custom Publishing, 2003.
  • [13] Bhote KR. World Class Quality: Design of Experiments Made Easier, More Cost Effective than SPC. Saranac Lake, first ed., Amacom Books, New York, American Management Association (AMACOM), 1998.
  • [14] Ramalingam P, Jahnavi B. Pharmaceutical Quality by Design. Principles and Applications. In: Beg S, Hasnain MdS (Eds). first ed., QbD Considerations for Analytical Development, Academic Press., Elsevier Inc., 2019, pp. 77-108.
  • [15] Quality Digest.Digging into DOE.https://www.qualitydigest.com/june01/html/doe.html. (accessed on 14 Feb 2014).
  • [16] Komati S, Swain S, Rao MEB, Jena BR, Unnam S, Dasi V. QbD-based design and characterization of mucoadhesive microspheres of quetiapine fumarate with improved oral bioavailability and brain biodistribution potential. Bull Fac Pharm Cairo Univ. 2018; 56: 129-145.
  • [17] European Commission. Annex 15. EU guide to good manufacturing practice: Qualification and validation. 2010; 4: 1–10
  • [18] Ravichandran V, Shalini S, Sundram KM, Rajak H. Validation of analytical methods-Strategies & importance. Int J Pharm Sci Res. 2010; 2: 340-345.
  • [19] Thompson M, Ellison SLR, Wood R. Harmonised guidelines for single laboratory validation of method of analysis. Pure Appl Chem. 2008; 74: 835-855.
  • [20] Validation of analytical procedure: Methodology Q2B. In: ICH Harmonized Tripartite Guidelines. Geneva, Switzerland. 1996. pp. 1-8.
  • [21] Sharma A, Sharma R. Validation of analytical procedures: A comparison of ICH Vs Pharmacopoiea (USP) Vs FDA. Int Res J Pharm. 2012; 3:39-42.Research Article
  • [22] Horwitz W. Evaluation of analytical methods used for regulation of foods and drugs. Anal. Chem. 1982; 54: 67A-76A.
  • [23] LC-MS method validation, robustness and ruggedness introduction. https://sisu.ut.ee/lcms_method_validation/10-ruggedness-robustness.(accessed on 9 Mar 2016).
  • [24] Stephan O. Krause. Good Analytical Method Validation Practice Deriving Acceptance Criteria for the AMV Protocol: Part.
  • [25] ICH, Q2B, “Validation of Analytical Procedures: Methodology.” Federal Register. Vol. 62. 1996.
  • [26] Blessy MN, Patel RD, Prajapati PN, and Agrawal YK. Development of forced degradation and stability indicating studies of drugs-A review. J Pharm Anal. 2014; 4: 159-165. [27] Jena BR, Panda SP, Kulandaivelu U, Alavala RR, Rao GSNK, Swain S, Ghose D, Pradhan DP. A QbD based study in development, optimization and forced degradation behaviour of Epinastine Hydrochloride in Metered dose inhaler by RP-HPLC. Int J Pharm Res. 2021; 13(1): 735–747.
  • [28] Requirements for the Registration of Pharmaceutical for Human Use: Validation of Analytical procedures, Text and Methodology, Q2 (R1), 2005.
  • [29] International Conference on Harmonization of Technical Requirements for the Registration of Pharmaceutical for Human Use: Stability Testing of New Drug Substances and Products Q1A (R2), 2005.

Yıl 2021, Cilt: 25 Sayı: 5, 689 - 701, 28.06.2025

Bikash Ranjan Jena Siva Prasad Panda Umasankar Kulandaivelu Rajasekhar Reddy Alavala G.s.n. Koteswara Rao Debashish Ghose Gurudutta Pattnaik Debi Prasad Pradhan

Öz

Kaynakça

  • [1] Abdine HH, Belal F, Al-Badr AA. Ipratropium Bromide: Physical Properties. Prof of Drug Subs Exc and Rel Methodol. 2003; 30: 59-83.
  • [2] Kasawar BG, Farooqui M. Development and Validation of a Stability Indicating RP-HPLC Method for the Simultaneous Determination of Related Substances of Albuterol Sulphate and Ipratropium Bromide in Nasal Solution. J Pharm Biomed Anal. 2010; 52: 19–29.
  • [3] Sowjanya G, Gowri SD, & Rao JVLNS. Development and validation of a new RPHPLC method for the simultaneous determination of albuterol sulphate and ipratropium bromide in nasal inhalations. Int Res J Pharm. 2018; 9:63-70.
  • [4] Orlandini S, Pinzauti S, & Furlanetto S. Application of quality by design to the development of analytical separation methods. Anal Bioanal Chem. 2013; 405: 443-450.
  • [5] Debrus D, Guillarme S.R. Improved quality-by-design compliant methodology for method development in reversed- phase liquid chromatography. J Pharm Biomed Anal. 2013; 84: 215-223.
  • [6] Ramalingam P, Kalva B, Yiragamreddy PR. Analytical Quality by Design: A Tool for Regulatory Flexibility and Robust Analytics. Int J Anal Chem. 2015; 10: 1-9.
  • [7] Swain S, Jena BR, Madugula D, and Beg S. Application of Quality by Design Paradigms for Development of Solid Dosage Forms. In: Beg S, Hasnain MS. (Eds). Pharmaceutical Quality by Design. Academic Press, 2019. pp.109-130.
  • [8] Li Y, Terfloth, GJ, Kord AS. A systematic approach to RP-HPLC method development in a pharmaceutical QbD environment. Ame Pharm Rev. 2009; 12: 01-09.
  • [9] Swain S, Parhi R, Jena BR, Babu SM. Quality by Design: Concept to Applications. Curr Drug Discov Technol. 2019; 16: 1-11.
  • [10] Sahu PK, Ramisetti NR, Swain S Patro CS, Panda J. An overview of experimental designs in HPLC method development and validation. J Pharm Biomed Anal. 2018; 147: 590-611.
  • [11] Jena BR, Panda SP, Umasankar K, Swain S, X Rao GSNK, Damayanthi D, Ghose D, Pradhan DP. Applications of QbD-based Software in Analytical Research and Development. Curr Pharm Anal. 2021; (17)1: 461-473.
  • [12] Allen TT, Design of Experiments and Other Six Sigma Related Methods Explained and Derived, Thomson Custom Publishing, 2003.
  • [13] Bhote KR. World Class Quality: Design of Experiments Made Easier, More Cost Effective than SPC. Saranac Lake, first ed., Amacom Books, New York, American Management Association (AMACOM), 1998.
  • [14] Ramalingam P, Jahnavi B. Pharmaceutical Quality by Design. Principles and Applications. In: Beg S, Hasnain MdS (Eds). first ed., QbD Considerations for Analytical Development, Academic Press., Elsevier Inc., 2019, pp. 77-108.
  • [15] Quality Digest.Digging into DOE.https://www.qualitydigest.com/june01/html/doe.html. (accessed on 14 Feb 2014).
  • [16] Komati S, Swain S, Rao MEB, Jena BR, Unnam S, Dasi V. QbD-based design and characterization of mucoadhesive microspheres of quetiapine fumarate with improved oral bioavailability and brain biodistribution potential. Bull Fac Pharm Cairo Univ. 2018; 56: 129-145.
  • [17] European Commission. Annex 15. EU guide to good manufacturing practice: Qualification and validation. 2010; 4: 1–10
  • [18] Ravichandran V, Shalini S, Sundram KM, Rajak H. Validation of analytical methods-Strategies & importance. Int J Pharm Sci Res. 2010; 2: 340-345.
  • [19] Thompson M, Ellison SLR, Wood R. Harmonised guidelines for single laboratory validation of method of analysis. Pure Appl Chem. 2008; 74: 835-855.
  • [20] Validation of analytical procedure: Methodology Q2B. In: ICH Harmonized Tripartite Guidelines. Geneva, Switzerland. 1996. pp. 1-8.
  • [21] Sharma A, Sharma R. Validation of analytical procedures: A comparison of ICH Vs Pharmacopoiea (USP) Vs FDA. Int Res J Pharm. 2012; 3:39-42.Research Article
  • [22] Horwitz W. Evaluation of analytical methods used for regulation of foods and drugs. Anal. Chem. 1982; 54: 67A-76A.
  • [23] LC-MS method validation, robustness and ruggedness introduction. https://sisu.ut.ee/lcms_method_validation/10-ruggedness-robustness.(accessed on 9 Mar 2016).
  • [24] Stephan O. Krause. Good Analytical Method Validation Practice Deriving Acceptance Criteria for the AMV Protocol: Part.
  • [25] ICH, Q2B, “Validation of Analytical Procedures: Methodology.” Federal Register. Vol. 62. 1996.
  • [26] Blessy MN, Patel RD, Prajapati PN, and Agrawal YK. Development of forced degradation and stability indicating studies of drugs-A review. J Pharm Anal. 2014; 4: 159-165. [27] Jena BR, Panda SP, Kulandaivelu U, Alavala RR, Rao GSNK, Swain S, Ghose D, Pradhan DP. A QbD based study in development, optimization and forced degradation behaviour of Epinastine Hydrochloride in Metered dose inhaler by RP-HPLC. Int J Pharm Res. 2021; 13(1): 735–747.
  • [28] Requirements for the Registration of Pharmaceutical for Human Use: Validation of Analytical procedures, Text and Methodology, Q2 (R1), 2005.
  • [29] International Conference on Harmonization of Technical Requirements for the Registration of Pharmaceutical for Human Use: Stability Testing of New Drug Substances and Products Q1A (R2), 2005.
Toplam 28 adet kaynakça vardır.

Ayrıntılar

Birincil Dil İngilizce
Konular Eczacılıkta Analitik Kimya
Bölüm Articles
Yazarlar

Bikash Ranjan Jena

Siva Prasad Panda

Umasankar Kulandaivelu

Rajasekhar Reddy Alavala

G.s.n. Koteswara Rao

Debashish Ghose

Gurudutta Pattnaik

Debi Prasad Pradhan

Yayımlanma Tarihi 28 Haziran 2025
Yayımlandığı Sayı Yıl 2021 Cilt: 25 Sayı: 5

Kaynak Göster

APA Jena, B. R., Panda, S. P., Kulandaivelu, U., Alavala, R. R., vd. (2025). Analytical QbD based systematic development of a novel RP-UHPLC method for the quantification of albuterol sulphate in its metered dose inhaler formulations. Journal of Research in Pharmacy, 25(5), 689-701.
AMA Jena BR, Panda SP, Kulandaivelu U, Alavala RR, Rao GK, Ghose D, Pattnaik G, Pradhan DP. Analytical QbD based systematic development of a novel RP-UHPLC method for the quantification of albuterol sulphate in its metered dose inhaler formulations. J. Res. Pharm. Temmuz 2025;25(5):689-701.
Chicago Jena, Bikash Ranjan, Siva Prasad Panda, Umasankar Kulandaivelu, Rajasekhar Reddy Alavala, G.s.n. Koteswara Rao, Debashish Ghose, Gurudutta Pattnaik, ve Debi Prasad Pradhan. “Analytical QbD Based Systematic Development of a Novel RP-UHPLC Method for the Quantification of Albuterol Sulphate in Its Metered Dose Inhaler Formulations”. Journal of Research in Pharmacy 25, sy. 5 (Temmuz 2025): 689-701.
EndNote Jena BR, Panda SP, Kulandaivelu U, Alavala RR, Rao GK, Ghose D, Pattnaik G, Pradhan DP (01 Temmuz 2025) Analytical QbD based systematic development of a novel RP-UHPLC method for the quantification of albuterol sulphate in its metered dose inhaler formulations. Journal of Research in Pharmacy 25 5 689–701.
IEEE B. R. Jena, S. P. Panda, U. Kulandaivelu, R. R. Alavala, G. K. Rao, D. Ghose, G. Pattnaik, ve D. P. Pradhan, “Analytical QbD based systematic development of a novel RP-UHPLC method for the quantification of albuterol sulphate in its metered dose inhaler formulations”, J. Res. Pharm., c. 25, sy. 5, ss. 689–701, 2025.
ISNAD Jena, Bikash Ranjan vd. “Analytical QbD Based Systematic Development of a Novel RP-UHPLC Method for the Quantification of Albuterol Sulphate in Its Metered Dose Inhaler Formulations”. Journal of Research in Pharmacy 25/5 (Temmuz 2025), 689-701.
JAMA Jena BR, Panda SP, Kulandaivelu U, Alavala RR, Rao GK, Ghose D, Pattnaik G, Pradhan DP. Analytical QbD based systematic development of a novel RP-UHPLC method for the quantification of albuterol sulphate in its metered dose inhaler formulations. J. Res. Pharm. 2025;25:689–701.
MLA Jena, Bikash Ranjan vd. “Analytical QbD Based Systematic Development of a Novel RP-UHPLC Method for the Quantification of Albuterol Sulphate in Its Metered Dose Inhaler Formulations”. Journal of Research in Pharmacy, c. 25, sy. 5, 2025, ss. 689-01.
Vancouver Jena BR, Panda SP, Kulandaivelu U, Alavala RR, Rao GK, Ghose D, Pattnaik G, Pradhan DP. Analytical QbD based systematic development of a novel RP-UHPLC method for the quantification of albuterol sulphate in its metered dose inhaler formulations. J. Res. Pharm. 2025;25(5):689-701.