Chandrasekaran Krishnan, Venkata Balarama Krishna Mullapudi, Nidhi Garg
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Chandrasekaran Krishnan*, Venkata Balarama Krishna Mullapudi, Nidhi Garg
National Centre for Compositional Characterization of Materials (NCCCM), Bhabha Atomic Research Centre, Department of Atomic Energy, Hyderabad - 500062, India.
Volume - 11,
Issue - 2,
Year - 2021
A single-step microwave assisted digestion (MWAD) procedure employing very dilute solutions of HNO3 was developed for the quantitative determination of bismuth in bismuth-containing pharmaceuticals by hydride generation-atomic fluorescence spectrometry (HG-AFS). Experimental parameters affecting MWAD process such as acid concentration (HNO3), digestion time and temperature were optimized to get quantitative recovery of bismuth. The studies indicated that the method is rapid (within 15 min) including cooling time and recovery > 98% was obtained using 10mL of 5% (v/v) HNO3 as digestion medium with ~0.1g of sample. The optimum microwave digestion parameters obtained were: temperature – 180oC, pressure – 25 bar and hold time - 10 min. A clear solution with negligible residue was obtained after microwave digestion. The digested sample solution was appropriately diluted with 2% (v/v) HCl for subsequent analysis by HG-AFS. The reproducibility, expressed as % RSD was lower than 2% for the allopathic medicine. Under optimal conditions, the limit of detection (LOD) for Bi was calculated to be 0.024mg/kg. The methodology was optimized using a bismuth-containing pharmaceutical – Pylobis, purchased from a local pharmacy. The optimized MWAD approach was further applied to few other bismuth-containing pharmaceutical products. The developed method has significant advantages when compared to the conventional hot-plate digestion methods reported for Bi-containing pharmaceuticals, employing large volumes of concentrated acids. These investigations revealed that the proposed MWAD method in combination with HG-AFS can be utilized for the rapid determination of Bi in pharmaceutical products on regular basis.
Cite this article:
Chandrasekaran Krishnan, Venkata Balarama Krishna Mullapudi, Nidhi Garg. Development of a Single-Step Microwave-Assisted Digestion Method using Dilute Nitric Acid for Determination of Bismuth in Bismuth-containing Pharmaceuticals by Hydride Generation-Atomic Fluorescence Spectrometry. Asian Journal of Pharmaceutical Analysis. 2021; 11(2):87-7. doi: 10.52711/2231-5675.2021.00017
Chandrasekaran Krishnan, Venkata Balarama Krishna Mullapudi, Nidhi Garg. Development of a Single-Step Microwave-Assisted Digestion Method using Dilute Nitric Acid for Determination of Bismuth in Bismuth-containing Pharmaceuticals by Hydride Generation-Atomic Fluorescence Spectrometry. Asian Journal of Pharmaceutical Analysis. 2021; 11(2):87-7. doi: 10.52711/2231-5675.2021.00017 Available on: https://ajpaonline.com/AbstractView.aspx?PID=2021-11-2-7
1. Salvador JAR, Figueiredo SAC, Pinto RMA and Silvestre SM. Bismuth compounds in medicinal chemistry. Future Medicinal Chemistry. 2012; 4(11): 1495–1523.
2. Das AK, Chakraborty R, Cervera ML and de la Guardia M. Analytical techniques for the determination of bismuth in solid environmental samples. TrAC Trends in Analytical Chemistry. 2006; 25(6): 599-608.
3. Briand GG and Burford N. Bismuth Compounds and Preparations with Biological or Medicinal Relevance. Chemical Reviews. 1999; 99(9): 2601-2657.
4. Thomas F, Bialek B and Hensel R. Medical Use of Bismuth: the Two Sides of the Coin. Journal of Clinical Toxicology. 2011; DOI:104172/2161-0495S3-004.
5. Hardman JG, Limbird LE, Molinoff PB, Ruddon RW and Gilman AG. Goodman Gilman’s The Pharmacological Basis of Therapeutics. 9th ed. New York: McGraw-Hill; 1999, p 3–63.
6. Kingston HM and Jassie LB. Introduction to Microwave Sample Preparation Theory Practice. American Chemical Society, Washington DC. 1988.
7. Bock RA. Handbook of Decomposition Methods in Analytical Chemistry. Wiley, New York. 1979.
8. Sulcek Z and Povondra P. Methods of Decomposition in Inorganic Analysis. CRC Press, FL Boca Raton. 1989.
9. Burns DT and Dangolle CDP. Spectrophotometric determination of bismuth in pharmaceutical samples by extraction of the tetraiodobismuthate (III) anion into propylene carbonate. Analytica Chimica Acta. 1997; 337(1): 113-116.
10. Agrawal K, Mundhara GL, Patel KS and Hoffmann P. Flow-Injection Analysis Spectrophotometric Determination of Bismuth in Environmental and Pharmaceutical Samples. Analytical Letters. 2004; 37(10): 2163-2174.
11. Cui F, Wang L and Cui Y. Determination of bismuth in pharmaceutical products using methyltriphenylphosphonium bromide as a molecular probe by resonance light scattering technique. Journal of Pharmaceutical and Biomedical Analysis. 2007; 43(3): 1033–1038.
12. Shamsipur M, Davarkhah R, Hassani R and Khanchi AR. Selective Ion Flotation Separation and Concentration of Ultra Trace Amounts of Bismuth Using Arsenazo III and Its Determination by Inductively Coupled Plasma-Atomic Emission Spectrometry. Separation Science and Technology. 2010; 45(9): 1340–1345.
13. Şahan S, Saçmacı Ş, Şahin U, Ülgen A and Kartal Ş. An on-line preconcentration/separation system for the determination of bismuth in environmental samples by FAAS. Talanta. 2010; 80(5): 2127–2131.
14. Yazdanipour A, Niazi A, Foladi SK and Tajik R. Determination of Trace Amounts of Bismuth in Pharmaceutical and Water by Adsorptive Cathodic Stripping Voltammetry in the Presence of Xylenol Orange. Oriental Journal of Chemistry 2012; 28(3): 1353-1359.
15. Pourreza N and Sheikhnajdi K. Multi-walled carbon nanotube modified with 1-buthyl 3-methyl imidazolium hexaflouro phosphate supported on sawdust as a selective adsorbent for solid phase extraction of Bi (III). Talanta 2012; 99: 507–511.
16. Rastegarzadeh S, Pourreza N and Larki A. Dispersive liquid–liquid microextraction for the microvolume spectrophotometric determination of bismuth in pharmaceutical and human serum samples. Analytical Methods. 2014; 6(10): 3500-3505.
17. Daşbaşı T, Kartal Ş, Saçmacı Ş and Ülgen A. Dispersive Liquid-Liquid Microextraction of Bismuth in Various Samples and Determination by Flame Atomic Absorption Spectrometry. Journal of Analytical Methods in Chemistry. 2016; DOI: 101155/6802646.
18. Verma C, Tapadia K, Soni AB and Sharma A. Determination of bismuth (III) in environmental and pharmaceutical samples using an organic reagent. Analytical Methods. 2017; 9(24): 3682-3688.
19. Kingston HM and Haswell SH. Microwave-Enhanced Chemistry Fundamentals, Sample preparation Applications. American Chemical Society, Washington DC. 1997.
20. Bendicho C, Lavilla I, Pena-Pereira F and Romero V. Green chemistry in analytical atomic spectrometry: review. Journal of Analytical Atomic Spectrometry. 2012; 27(11): 1831–1857.
21. Rocha DL, Batista AD, Rocha FRP, Donati GL and Nóbrega JA. Greening sample preparation in inorganic analysis. TrAC Trends in Analytical Chemistry. 2013; 45: 79–92.
22. Tobiszewski M. Metrics for green analytical chemistry. Analytical Methods. 2016; 8(15): 2993–2999.
23. Pinheiro FC, Babos DV, Barros AI, Pereira-Filho ER and Nóbrega JA. Microwave-assisted digestion using dilute nitric acid solution and investigation of calibration strategies for determination of As, Cd, Hg and Pb in dietary supplements using ICP-MS. Journal of Pharmaceutical and Biomedical Analysis. 2019; 174(10): 471–478.
24. Tarantino TB, Barbosa IS, Lima D de C, Pereira M de G, Teixeira LSG and Korn MGA. Microwave-Assisted Digestion Using Diluted Nitric Acid for Multi-element Determination in Rice by ICP OES and ICP-MS. Food and Analytical Methods. 2017; 10: 1007–1015.
25. Muller ALH, Muller EI, Barin JS and Flores EMM. Microwave-assisted digestion using diluted acids for toxic element determination in medicinal plants by ICP-MS in compliance with United States pharmacopeia requirements. Analytical Methods. 2015; 7(12): 5218–5225.
26. Bizzi CA, Nóbrega JA, Barin JS, Oliveira JSS, Schmidt L and Mello PA. Effect of Simultaneous Cooling on Microwave-Assisted Wet Digestion of Biological Samples with Diluted Nitric Acid and O2 pressure. Analytica Chimica Acta. 2014; 837: 16–22.
27. Bizzi CA, Barin JS, Müller EI, Schmidt L, Nóbrega JA and Flores EMM. Evaluation of oxygen pressurized microwave-assisted digestion of botanical materials using diluted nitric acid. Talanta 2011; 83(5): 1324–1328.
28. Bizzi CA, Flores ELM, Nóbrega JA, Oliveira JSS, Schmidt L and Mortari SR. Evaluation of a digestion procedure based on the use of diluted nitric acid solutions and H2O2 for the multielement determination of whole milk powder and bovine liver by ICP-based techniques. Journal of Analytical Atomic Spectrometry. 2014; 29(2): 332–338.
29. Barela PS, Silva NA, Pereira JSF, Marques JC, Rodrigues LF and Moraes DP. Microwave-assisted digestion using diluted nitric acid for further trace elements determination in biodiesel by SF-ICP-MS. Fuel. 2017; 204: 85–90.
30. Pereira RM, Crizel MG, Novo DLaR, dos Santos CMM and Mesko MF. Multitechnique determination of metals and non-metals in sports supplements after microwave-assisted digestion using diluted acid. Microchemical Journal. 2019; 145: 235–241.
31. Pinheiro FC, Barros AI and Nóbrega JA. Microwave-assisted sample preparation of medicines for determination of elemental impurities in compliance with United States Pharmacopeia: How simple can it be? Analytica Chimica Acta. 2019; 1065: 1-11.
32. Flores EMM. Microwave-assisted sample preparation for trace element determination. Elsevier, Amsterdam. 2014.
33. Mester Z and Sturgeon R. Sample preparation for trace element analysis. Vol XLI. Elsevier, Amsterdam. 2003.
34. Barin JS, Mello PA, Mesko MF, Duarte FA and Flores EMM. Determination of elemental impurities in pharmaceutical products and related matrices by ICP-based methods: a review. Analytical Bioanalytical Chemistry. 2016; 408: 4547–4566.
35. Matusiewicz H. Wet digestion methods. In Sample preparation for trace element analysis, Edited by Mester Z and Sturgeon R. vol XLI. Elsevier, Amsterdam. 2003; pp. 193–234.
36. Balarama Krishna MV, Chandrasekaran K, Venkateswarlu G and Karunasagar D. Development of a simple and rapid microwave-assisted extraction method using very dilute solutions of perchloric acid and hydrogen peroxide for the multi-elemental analysis of food materials by ICP-OES: A green analytical method. Microchemical Journal. 2019; 146: 807–817.
37. Bizzi CA, Flores EMM, Picoloto RS, Barin JS and Nóbrega JA. Microwave-assisted digestion in closed vessels: effect of pressurization with oxygen on digestion process with diluted nitric acid. Analytical Methods. 2010; 2(6): 734–738.
38. Bizzi CA, Flores EMM, Barin JS, Garcia EE and Nóbrega JA. Understanding the process of microwave-assisted digestion combining diluted nitric acid and oxygen as auxiliary reagent. Microchemical Journal. 2011; 99(2): 193-196.
39. Castro JT, Santos EC, Santos WPC, Costa LM, Korn M, Nóbrega JA and Korn MGA. A critical evaluation of digestion procedures for coffee samples using diluted nitric acid in closed vessels for inductively coupled plasma optical emission spectrometry. Talanta. 2009; 78(4-5): 1378–1382.
40. Gouveia ST, Silva FV, Costa LM, Nogueira ARA and Nóbrega JA. Determination of residual carbon by inductively-coupled plasma optical emission spectrometry with axial and radial view configurations. Analytica Chimica Acta. 2001; 445(2): 269-275.
41. Kılınç E and Aydın F. Optimization of Continuous Flow Hydride Generation Inductively Coupled Plasma Optical Emission Spectrometry for Sensitivity Improvement of Bismuth. Analytical Letters. 2012; 45(17): 2623-2636.
42. Muller ALH, Oliveira JSS, Mello PA, Muller EI and Flores EMM. Study and determination of elemental impurities by ICP-MS in active pharmaceutical ingredients using single reaction chamber digestion in compliance with USP requirements. Talanta. 2015; 136: 161–169.
43. Balaram V. Recent advances in the determination of elemental impurities in pharmaceuticals – Status, challenges and moving frontiers. TrAC Trends in Analytical Chemistry. 2016; 80: 83–95.
44. Alonso A, Almendral MJ, Báez MD, Porras MJ, Lavín FL and de María CG. Determination of bismuth in pharmaceutical products using liquid–liquid extraction in a flow injection system. Analytica Chimica Acta. 2000; 408(1-2): 129–133.