DETERMINATION OF TOXIC HEAVY METALS IN CHOLIC ACID USING QUADRUPOLE INDUCTIVELY COUPLED PLASMA MASS SPECTROMETRY

Thakar Meet Kumar; Suthar Vaishali; Sheth Jateen; Indra Neel Pulidindi; SHARMA PANKAJ

doi:10.22159/ajpcr.2023.v16i12.47366

Authors

Thakar Meet Kumar Department of Applied Chemistry, Faculty of Technology and Engineering, The Maharaja Sayajirao University of Baroda, Vadodara, Gujarat, India.
Suthar Vaishali Department of Applied Chemistry, Faculty of Technology and Engineering, The Maharaja Sayajirao University of Baroda, Vadodara, Gujarat, India.
Sheth Jateen School of Liberal Studies and Education, Navrachana University, Vadodara, Gujarat, India.
Indra Neel Pulidindi School of Sciences, GSFC University, Vadodara, Gujarat, India.
SHARMA PANKAJ Department of Applied Chemistry, Faculty of Technology and Engineering, The Maharaja Sayajirao University of Baroda, Vadodara, Gujarat, India. https://orcid.org/0000-0002-7467-6471

DOI:

https://doi.org/10.22159/ajpcr.2023.v16i12.47366

Keywords:

Cholic acid, Metal impurities, Heavy metals, Analytical method development and validation, Microwave acid-digestion, Quadrupole inductively coupled plasma mass spectrometry

Abstract

Objective: The information on the presence of toxic heavy metals in pharmaceutical starting materials and finished product is very crucial from the viewpoint of human life and its hazardous impact on the worldwide environment. The present work deals with the detailed quantification of the toxic heavy metals, namely, V, Co, Ni, Cd, Hg, Pb, and As, present in colic acid using quadrupole inductively coupled plasma mass spectrometry (Q-ICPMS) with prior microwave-assisted digestion. Moreover, the preliminary characterization of commercially available cholic acid by FT-IR, NMR (1H and 13C), SEM-EDAX has also been carried out.

Methods: Cholic acid of synthesis grade, Nitric acid (65%) AR. grade, ethylene diamine tetra acetic acid sodium salt AR grade, and certified reference metal stock standard solutions (1000 mg/L) of multiple elements prepared in 2–3% HNO3 of analytical grade were purchased from Merck (Darmstadt, Germany). All the samples were treated with nitric acid and microwave-assisted digestion. For the accurate determination of the elemental amount, various digested solutions and post-digestion diluents were tested. The linearity, accuracy, precision, limit of detection (LOD), and limit of quantification (LOQ) of the analytical technique were evaluated in accordance with the United States Pharmacopoeia 233 standard.

Results and Discussion: The Q-ICPMS-based analytical method was validated for specificity, LOD, LOQ, linearity, accuracy, precision, and uncertainty. The estimated detection limits of the toxic heavy metals in cholic acid were in the range 2–180 μg/L. The quantification limits were in the range of 1.5–60 μg/L. Mean recoveries±standard deviations at different spiking levels were in the range 75.3±2.1–104.9±8.5%. The coefficients of variation were in the range of 0.5–8.1%.

Conclusion: The precision of the analytical method, in terms of relative standard deviation, was below 1.95%. The uncertainty in the quantification of all the validated elements was found to be ≤1.70% for Sample 1.

Downloads

Download data is not yet available.

References

Zhang JW, Luo JT, Zhu XX, Junk MJ, Hinderberger D. Molecular pockets derived from cholic acid as chemosensors for metal ions. Langmuir 2010;26:2958-62.

Zhang J, Junk MJ, Hinderberger D, Zhu XX. 1, 2, 3-triazole-containing molecular pockets derived from cholic acid: The influence of structure on host-guest coordination properties. Langmuir 2010;26:13415-21.

Blazorics A, Szentmihalyi K, Rapavi E, Feher E, Vinkler P. Accumulation of toxic elements in liver and bile in hyperlipidemy. Trace Elem Electrolytes 2003;20:211-6.

Annadhasan M, Kasthuri J, Rajendran N. A facile sunlight-induced synthesis of pheylalanine-conjugated cholic acid-stabilized silver and gold nanoparticles for colorimetric detection of toxic Hg2+, Cr6+, and Pb2+ ions. Chemistryselect 2019;4:655767.

Ghuniem MM, Khorshed MA, Souaya ER. Method validation for direct determination of some trace and toxic elements in soft drinks by inductively coupled plasma mass spectrometry. Int J Environ Anal Chem 2019;99:515-40.

Jin D, Li L, Dong W, Zhu XY, Xia XJ, Wang RY, et al. Research on transfer rate of heavy metals and harmful elements in traditional chinese medicine extraction and refining processes and product health risk assessment. Bio Trace Elem Res 2022;200:1956-64.

Abernethy DR, DeStefano AJ, Cecil TL, Zaidi K, Williams RL, USP Metal Impurities Advisory Panel. Metal impurities in food and drugs. Pharm Res 2010;27:750-5.

Balali-Mood M, Naseri K, Tahergorabi Z, Khazdair MR, Sadeghi M. Toxic mechanisms of five heavy metals: Mercury, lead, chromium, cadmium, and arsenic. Front Pharmacol 2021;12:643972.

Mousavi SR, Balali-Mood M, Riahi-Zanjani B, Yousefzadeh H, Sadeghi M. Concentrations of mercury, lead, chromium, cadmium, arsenic and aluminum in irrigation water wells and wastewaters used for agriculture in Mashhad, Northeastern. Iran Int J Occup Environ Med 2013;4:80-6.

Tchounwou PB, Yedjou CG, Patlolla AK, Sutton DJ. Heavy metals toxicity and the environment. Exp Suppl 2012;101:133-64.

Bradl H. Heavy Metals in the Environment: Origin, Interaction and Remediation. London: Academic Press; 2002.

Mohamed R, Zainudin BH, Yaakob AS. Method validation and determination of heavy metals in cocoa beans and cocoa products by microwave assisted digestion technique with inductively coupled plasma mass spectrometry. Food Chem 2020;303:125392.

Ghuniem MM, Khorshed MA, Souaya ER. Optimization and validation of an analytical method for the determination of some trace and toxic elements in canned fruit juices using quadrupole inductively coupled plasma mass spectrometer. J AOAC Int 2019;102:262-9.

Rao RN, Talluri MV. An overview of recent applications of inductively coupled plasma-mass spectrometry (ICP-MS) in determination of inorganic impurities in drugs and pharmaceuticals. J Pharm Biomed Anal 2007;43:1-13.

Katakam LN, Aboul-Enein HY. Elemental impurities determination by ICP-AES/ICP-MS: A review of theory, interpretation of concentration limits: Analytical method development challenges and validation forms. Curr Pharm Anal 2020;16:392-403.

Vessman J, Stefan RI, Von Staden JF, Danzer K, Lindner WG, Burns DT, et al. International union of pure and applied chemistry. Pure Appl Chem 2001;73:1381-6.

Veeramachaneni M, Jayavarapu KR. Development and validation of new ICP-OES analytical technique to quantify the contents of copper, magnesium & zinc in escitalopram oxalate. J Adv Pharm Educ Res 2013;3:516-23.

Shrivastava A, Gupta VB. Methods for the determination of limit of detection and limit of quantitation of the analytical methods. Chron Young Sci 2011;2:21-5.

Carr GP, Wahlich JC. A practical approach to method validation in pharmaceutical analysis. J Pharm Biomed Anal 1990;8:613-8.

Lecomte F, Hubert C, Demarche S, De Bleye C, Dispas A, Jost M, et al. Comparison of the quantitative performances and measurement uncertainty estimates obtained during method validation versus routine applications of a novel hydrophilic interaction chromatography method for the determination of cidofovir in human plasma. J Pharm Biomed Anal 2012;57:153-65.

Shabir GA, Lough WJ, Arain SA, Bradshaw TK. Evaluation and application of best practice in analytical method validation. J Liquid Chromatogr Relat Technol 2007;30:311-33.

Bruce P, Minkkinen P, Riekkola ML. Practical method validation: Validation sufficient for an analysis method. Mikrochim Acta 1998;128:93-106.

Wilschefski SC, Baxter MR. Inductively coupled plasma mass spectrometry: Introduction to analytical aspects. Clin Biochem Rev 2019;40:115-33.