METHOD DEVELOPMENT AND VALIDATION OF CEFOPERAZONE AND SULBACTAM IN DRIED BLOOD SPOTS BY HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY PHOTODIODE ARRAY DETECTOR

Authors

  • DIAN PERMATA Faculty of Pharmacy, Universitas Indonesia, 16424 Depok, West Java, Indonesia https://orcid.org/0000-0002-2932-9243
  • YAHDIANA HARAHAP Bioavailability and Bioequivalence Laboratory, Faculty of Pharmacy, Universitas Indonesia, 16424 Depok, West Java, Indonesia, Faculty of Military Pharmacy, Republic of Indonesia Defense University, Bogor, 16810, West Java, Indonesia https://orcid.org/0000-0002-7217-7900
  • DELLY RAMADON Laboratory of Pharmaceutics and Pharmaceutical Technology, Faculty of Pharmacy, Universitas Indonesia, 16424 Depok, West Java, Indonesia https://orcid.org/0000-0002-2847-9610

DOI:

https://doi.org/10.22159/ijap.2022v14i5.45078

Keywords:

Cefoperazone, Sulbactam, Dried blood spots (DBS), HPLC

Abstract

Objective: The primary purpose of this research was to develop a simple, precise, fast, and accurate method for measuring cefoperazone and sulbactam simultaneously in dried blood spots (DBS) using HPLC PDA.

Methods: A simplified analytical method for quantifying cefoperazone and sulbactam in DBS samples using a High-Performance Liquid Chromatography photodiode array detector with isocratic elution was developed and validated. The best chromatographic conditions were obtained by using a reversed-phase column (250 x 4.6 mm; 5 mm); phosphate buffer 10 mmol pH 3.2–acetonitrile (83:17, v/v) as a mobile phase; a flow rate of 1.0 ml/min; a column temperature of 35 °C; a photodiode array detector at 210 nm, and cefuroxime as internal standard. Samples were prepared by liquid-liquid extraction with 100 ml hydrochloric acid 0.5 mol/l and 1000 ml ethyl acetate, evaporated with nitrogen and reconstituted with 100 mL phosphate buffer–acetonitrile (4:1).

Results: The total chromatography run time was 15 min, and the elution times for sulbactam, cefoperazone, and IS (cefuroxime) were 3.46, 10.221, and 6.987 min, respectively. A linear response function was established at 0.5-30 mg/ml with (r) 0.995 for sulbactam and 2.5-250 mg/ml with (r) 0.999 for cefoperazone in dried blood spots. The lower limit quantification (LLOQ) concentration of sulbactam 1 mg/ml and cefoperazone were 5 mg/ml.

Conclusion: This method has successfully fulfilled the validation requirement referring to the 2011 EMA and 2018 FDA guidelines.

Downloads

Download data is not yet available.

References

Kyriakidis I, Vasileiou E, Pana ZD, Tragiannidis A. Acinetobacter baumannii antibiotic resistance mechanisms. Pathogens. 2021;10(3):1-31. doi: 10.3390/pathogens10030373, PMID 33808905.

Liu X, Wu X, Tang J, Zhang L, Jia X. Trends and development in the antibiotic-resistance of Acinetobacter baumannii: A scientometric research study (1991-2019). Infect Drug Resist. 2020;13:3195-208. doi: 10.2147/IDR.S264391, PMID 32982334.

Purba AK, Ascobat P, Muchtar A, Wulandari L, Rosyid AN, Purwono PB. Multidrug-resistant infections among hospitalized adults with community-acquired pneumonia in an Indonesian tertiary referral hospital. Infect Drug Resist. 2019;12:3663-75. doi: 10.2147/IDR.S217842, PMID 31819549.

Xie J, Wang Y, Zheng X, Yang Q, Wang T, Zou Y. Modeling and forecasting Acinetobacter baumannii resistance to set appropriate use of cefoperazone-sulbactam: results from trend analysis of antimicrobial consumption and development of resistance in a tertiary care hospital. Am J Infect Control. 2015;43(8):861-4. doi: 10.1016/j.ajic.2015.04.197, PMID 26033693.

Cazorla Reyes R, Romero Gonzalez R, Frenich AG, Rodriguez Maresca MA, Martinez Vidal JL. Simultaneous analysis of antibiotics in biological samples by ultra-high-performance liquid chromatography-tandem mass spectrometry. J Pharm Biomed Anal. 2014;89:203-12. doi: 10.1016/ j.jpba.2013.11.004, PMID 24291112.

Zhou Y, Zhang J, Guo B, Yu J, Shi Y, Wang M. Liquid chromatography/tandem mass spectrometry assay for the simultaneous determination of cefoperazone and sulbactam in plasma and its application to a pharmacokinetic study. J Chromatogr B Analyt Technol Biomed Life Sci. 2010;878(30):3119-24. doi: 10.1016/j.jchromb.2010.09.021, PMID 20971044.

Korake S, Pawar A, Surywanshi S, Bothiraja C, Pawar A. High-performance liquid chromatography for the simultaneous estimation of cefoperazone and sulbactam in rat plasma and its importance in therapeutic drug monitoring. Int J Pharm Pharm Sci. 2020;12(441):92-7. doi: 10.22159/ijpps.2020v12i10.38638.

Denniff P, Spooner N. Volumetric absorptive microsampling: A dried sample collection technique for quantitative bioanalysis. Anal Chem. 2014;86(16):8489-95. doi: 10.1021/ac5022562, PMID 25058158.

Pedersen L, Andersen Ranberg K, Hollergaard M, Nybo M. Quantification of multiple elements in dried blood spot samples. Clin Biochem. 2017;50(12):703-9. doi: 10.1016/j.clinbiochem.2017.01.010, PMID 28122197.

Schellinger AP, Carr PW. Isocratic and gradient elution chromatography: A comparison in terms of speed, retention reproducibility and quantitation. J Chromatogr A. 2006;1109(2):253-66. doi: 10.1016/j.chroma.2006.01.047, PMID 16460742.

Pei Q, Yang GP, Li ZJ, Peng XD, Fan JH, Liu ZQ. Simultaneous analysis of amoxicillin and sulbactam in human plasma by HPLC-DAD for assessment of bioequivalence. J Chromatogr B Analyt Technol Biomed Life Sci. 2011;879(21):2000-4. doi: 10.1016/j.jchromb.2011.05.021, PMID 21680260.

Food and Drug Administration. Guidance for Industry: bioanalytical method validation. Rockville, MD: United States Department of Health and Human Services, Food and Drug Administration; 2018. p. 1-41.

Tijare LK, Nt R, Un M. A review on bioanalytical method development and validation. Asian J Pharm Clin Res. 2016;9(9):6-10. doi: 10.22159/ajpcr.2016.v9s3.14321.

EMEA. Guideline on bioanalytical method validation, Sciences Medicines Health. London: European Medicines Agency; 2011.

Lakka SN, Kuppan C. Principles of chromatography method development. In: Boldura OM, Balta C, Awwad NS, editors. Biochemical analysis tools methods for bio-molecules studies. London: Intech Open; 2012. p. 161-82.

Sabir AM, Moloy M, Bhasin PS. HPLC method development and validation: a review. Int Res J Pharm. 2016;4(4):39-46. doi: 10.7897/2230-8407.04407.

Published

07-09-2022

How to Cite

PERMATA, D., HARAHAP, Y., & RAMADON, D. (2022). METHOD DEVELOPMENT AND VALIDATION OF CEFOPERAZONE AND SULBACTAM IN DRIED BLOOD SPOTS BY HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY PHOTODIODE ARRAY DETECTOR. International Journal of Applied Pharmaceutics, 14(5), 214–219. https://doi.org/10.22159/ijap.2022v14i5.45078

Issue

Section

Original Article(s)