Validation of An Efficient 2D-HPLC Method for The Determination of Pentazocine

Maha Thamer Ahmed

doi:10.22146/ijc.87947

Validation of An Efficient 2D-HPLC Method for The Determination of Pentazocine

https://doi.org/10.22146/ijc.87947

Maha Thamer Ahmed^(1*)

(1) Directorate of Education Salah AL-Din, Education Department of Balad, Salah AL-Din 34000, Iraq
(*) Corresponding Author

Abstract

Pentazocine is an opioid analgesic used to treat moderate to severe pains. The real analysis for the pharmaceutical products containing pentazocine is basically to ensure the correct dose and patient safety. This study developed and validated an improved high-performance liquid chromatography (HPLC) method in the selective and accurate quantification of pentazocine. Two-dimensional (2D) HPLC technique is employed to enhance the resolution and selectivity compared to conventional HPLC methods. The 2D-HPLC instrumentation consists of two C18 columns coupling with a switching valve to capture fractions from the first column, which is analyzed in the second column. The mobile phase was optimized to 45% acetonitrile and 55% water with 0.1% phosphoric acid. The method was validated in the International Conference on Harmonization guidelines and shows excellent linearity (R²=0.998), limit of detection of 1.58 μg/L, accuracy of 97.70–102.50%, and precision by relative standard deviation (RSD) of 1.02–4.20%. Selectivity was verified in resolving pentazocine from paracetamol, caffeine, ibuprofen, and oxycodone in laboratory mixtures. The utility of the 2D-HPLC method was demonstrated by accurate quantification of pentazocine in pharmaceutical injections and tablets unaffected in excipients. This research provides a rich validating technique to enhance the quality control testing of pharmaceuticals containing pentazocine.

Keywords

pentazocine; quantification; selectivity; validation; 2D-HPLC

Full Text:

Full Text PDF

References

[1] Goldstein, G., 1985, Pentazocine, Drug Alcohol Depend., 14 (3-4), 313–323.‏

[2] Ansari, A., Mahmood, T., Bagga, P., Ahsan, F., Shamim, A., Ahmad, S., Shariq, M., and Parveen, S., 2021, Areca catechu: A phytopharmacological legwork, Food Front., 2 (2), 163–183.‏

[3] Huang, H., Bai, X., Zhang, K., Guo, J., Wu, S., and Ouyang, H., 2022, Antinociceptive effects and interaction mechanisms of intrathecal pentazocine and neostigmine in two different pain models in rats, Pain Res. Manage., 18, 4819910.

[4] Mahapatra, S.J., Jain, S., Bopanna, S., Gupta, S., Singh, P., Trikha, A., Sreenivas, V., Shalimar, S., and Garg, P.K., 2019, Pentazocine, a kappa-opioid agonist, is better than diclofenac for analgesia in acute pancreatitis: A randomized controlled trial, Am. J. Gastroenterol., 114 (5), 813–821.‏

[5] Gress, K., Charipova, K., Jung, J.W., Kaye, A.D., Paladini, A., Varrassi, G., Viswanath, O., and Urits, I., 2020, A comprehensive review of partial opioid agonists for the treatment of chronic pain, Best Pract. Res., Clin. Anaesthesiol., 34 (3), 449–461.‏

[6] Espro, C., Paone, E., Mauriello, F., Gotti, R., Uliassi, E., Bolognesi, M.L., Rodríguez-Padrón, D., and Luque, R., 2021, Sustainable production of pharmaceutical, nutraceutical and bioactive compounds from biomass and waste, Chem. Soc. Rev., 50 (20), 11191–11207.‏

[7] Ozawa, S., Chen, H.H., Lee, Y.F.A., Higgins, C.R., and Yemeke, T.T., 2022, Characterizing medicine quality by active pharmaceutical ingredient levels: A systematic review and meta-analysis across low-and middle-income countries, Am. J. Trop. Med. Hyg., 106 (6), 1778–1790.‏

[8] Jabar, A., Madni, A., Bashir, S., Tahir, N., Usman, F., Rahim, M.A., Jan, N., Shah, H., Khan, A., and Khan, S., 2021, Statistically optimized pentazocine loaded microsphere for the sustained delivery application: Formulation and characterization, PLoS One, 16 (4), e0250876.‏

[9] Mukherjee, P.K., Banerjee, S., and Kar, A., 2018, Exploring synergy in ayurveda and traditional Indian systems of medicine, Synergy, 7, 30–33.‏

[10] Kumar, S.V., Damodar, G., Ravikanth, S., and Vijayakumar, G., 2012, An overview on infectious disease, Indian J. Pharm. Sci. Res., 2 (2), 63–74.‏

[11] Shaikh, T., Nafady, A., Talpur, F.N., Sirajuddin, S., Agheem, M.H., Shah, M.R., Sherazi, S.T.H., Soomro, R.A., and Siddiqui, S., 2015, Tranexamic acid derived gold nanoparticles modified glassy carbon electrode as sensitive sensor for determination of nalbuphine, Sens. Actuators, B, 211, 359–369.‏

[12] Elqudaby, H.M., Hendawy, H.A., Souaya, E.R., Mohamed, G.G., and Eldin, G.M.G., 2016, Utility of activated glassy carbon and pencil graphite electrodes for voltammetric determination of nalbuphine hydrochloride in pharmaceutical and biological fluids, Int. J. Electrochem., 2016, 8621234.‏

[13] Volz, M.R., and Moosmann, B., 2022, Development of a non-radioactive mass spectrometry-based binding assay at the μ-opioid receptor and its application for the determination of the binding affinities of 17 opiates/opioids as well as of the designer opioid isotonitazene and five further 2-benzylbenzimidazoles, Anal. Chim. Acta, 1219, 339978.‏

[14] Aljeboree, A.M., 2020, Spectrophotometric and colorimetric determination of pharmaceutical by oxidative coupling reaction: A review, Syst. Rev. Pharm., 11 (4), 609–615.‏

[15] El-Didamony, A.M., Saad, M.Z., and Saleem, N.O., 2015, Spectrophotometric determination of some analgesic drugs in pharmaceutical formulations using N-bromosuccinimide as an oxidant, J. Assoc. Arab Univ. Basic Appl. Sci., 17, 43–50.‏

[16] Jain, R., Ghosh, S., and Saifi, N., 2022, An efficient method for simultaneous detection of Pheniramine, Pentazocine and cotinine in urine by Gas Chromatography in De-addiction program, Addict. Health, 14 (2), 96–104.‏

[17] Chan, K.H., Hsu, M.C., and Chu, W.L., 2007, Determination of pentazocine in urine by gas chromatography-mass spectrometry, J. Food Drug Anal., 15 (3), 228–232.‏

[18] Saito, K., Nishiyama, R., and Ito, R., 2021, Simultaneous quantitative screening for pain medications in serum by high-performance liquid chromatography/time-of-flight mass spectrometry with solid-phase dispersive extraction, Chromatography, 42 (2), 83–90.

[19] Miwa, D., Kitamura, Y., Kozaka, T., Shigeno, T., Ogawa, K., Taki, J., Kinuya, S., and Shiba, K., 2020, (−)‐o‐[¹¹C] methyl‐trans‐decalinvesamicol ((−)‐[¹¹C] OMDV) as a PET ligand for the vesicular acetylcholine transporter, Synapse, 74 (11), e22176.‏

[20] Alnedawi, Z., Hassan, A.M., Hadi, H., and Shabana, A., 2022, Development HPLC technique for determining Oxymetazoline and Isoxspurine in pharmaceutical formulations, Egypt. J. Chem., 65 (11), 779–784.‏

[21] Liang, L., Duan, W., Zhao, C., Zhang, Y., and Sun, B., 2022, Recent development of two-dimensional liquid chromatography in food analysis, Food Anal. Methods, 15 (5), 1214–1225.‏

[22] Qi, D., Fei, T., Liu, H., Yao, H., Wu, D., and Liu, B., 2017, Development of multiple heart-cutting two-dimensional liquid chromatography coupled to quadrupole-orbitrap high resolution mass spectrometry for simultaneous determination of aflatoxin B1, B2, G1, G2, and ochratoxin A in snus, a smokeless tobacco product, J. Agric. Food Chem., 65 (45), 9923–9929.‏

[23] Guo, P., Xu, X., Xian, L., Ge, Y., Luo, Z., Du, W., Jing, W., Zeng, A., Chang, C., and Fu, Q., 2016, Development of molecularly imprinted column-on line-two-dimensional liquid chromatography for rapidly and selectively monitoring estradiol in cosmetics, Talanta, 161, 830–837.‏

[24] Stoll, D.R., and Carr, P.W., 2017, Two-dimensional liquid chromatography: A state of the art tutorial, Anal. Chem., 89 (1), 519–531.‏

[25] Dixon, J.R., 1999, The international conference on harmonization good clinical practice guideline, Qual. Assur., 6 (2), 65–74.‏

[26] Singh, J., 2015, International conference on harmonization of technical requirements for registration of pharmaceuticals for human use, J. Pharmacol. Pharmacother., 6 (3), 185–187.‏

[27] Alam, P., Shakeel, F., Ali, A., Alqarni, M.H., Foudah, A.I., Aljarba, T.M., Alkholifi, F.K., Alshehri, S., Ghoneim, M.M., and Ali, A., 2022, Simultaneous determination of caffeine and paracetamol in commercial formulations using greener normal-phase and reversed-phase HPTLC methods: A contrast of validation parameters, Molecules, 27 (2), 405.‏

[28] Borahan, T., Unutkan, T., Şahin, A., and Bakırdere, S., 2019, A rapid and sensitive reversed phase‐HPLC method for simultaneous determination of ibuprofen and paracetamol in drug samples and their behaviors in simulated gastric conditions, J. Sep. Sci., 42 (3), 678–683.‏

[29] Coles, R., Kushnir, M.M., Nelson, G.J., McMillin, G.A., and Urry, F.M., 2007, Simultaneous determination of codeine, morphine, hydrocodone, hydromorphone, oxycodone, and 6-acetylmorphine in urine, serum, plasma, whole blood, and meconium by LC-MS-MS, J. Anal. Toxicol., 31 (1), 1–14.‏

[30] Papatheocharidou, C., and Samanidou, V., 2023, Two-dimensional high-performance liquid chromatography as a powerful tool for bioanalysis: The paradigm of antibiotics, Molecules, 28 (13), 5056.

DOI: https://doi.org/10.22146/ijc.87947