Capsaicin determination from pain patch for the calculation of Scoville heat units by gas chromatography-mass spectrometry

Year 2021, Volume: 51 Issue: 3, 386 - 391, 29.12.2021

İbrahim Daniş Durişehvar Ünal

Abstract

Background and Aims: A sensitive, accurate and precise method has been developed for the determination of Capsaicin from pain patches by Gas chromatography Mass Spectrometry (GC-MS). Capsaicin has irritant effects in high concentrations, so these effects can be minimized by knowing the amount present in pain patches for the efficacy and safety of patches. Methods: Capsaicin was extracted by using liquid-liquid extraction from patches. The Gas Chromatographic separation was performed by using 5% diphenyl 95% dimethylpolysiloxane column with high a purity 2 mL/min flow rate helium gas. The separation was made with a gradient oven temperature program. The oven temperature started at 250°C and was increased to 275°C at 10°C.min-1 ramp rate and held at 275°C for 2.5 min. The injection port was adjusted at 300°C and a split injection mode was used. The analysis was carried out in a split mode of 5:1. MS ionization potential was determined at 70 eV. Results: The calibration curve was found to be linear in the range 5 - 50 μg/mL. The limits of detection and quantification for capsaicin was found to be 3.46 μg/mL and 5 μg/mL, respectively. The method developed was validated and successfully applied to the patch analysis. Conclusion: This method is simple, reproducible, and can be used safely for the routine analysis of Capsaicin without derivatization. This study has the potential how to calculate the Scoville Heat Units (SHU) of pain patches that contain Capsaicin. The amount of Capsaicin in the pain patch, its irritant effects, and its efficacy and safety appear to be low when evaluated by the SHU.

Keywords

Capsicum, Capsaicin, pain patch, gas chromatography-mass spectrometry, Scoville

Supporting Institution

This study was supported by İstanbul University, Scientific Research Projects.

Project Number

55974

Thanks

We would like to thank Prof. Dr. Süleyman Patır for providing us Capsaicine standard.

References

• • Anand, P., & Bley, K. (2011). Topical capsaicin for pain management: therapeutic potential and mechanisms of action of the new high-concentration capsaicin 8% patch. British Journal of Anaesthesia, 107(4), 490–502. https://doi.org/10.1093/bja/aer260
• • Ashwini, D., Usha, S. G., Ajitha, A., & Rao, V. U. M. (2015). Extraction of capsaicin from capsicum frutescens. l and its estimation by rp-hplc method. World Journal of Pharmacy and Pharmaceutical Sciences, 4(9), 839-848.
• • Baranidharan, G., Das, S., & Bhaskar, A. (2013). A review of the high-concentration capsaicin patch and experience in its use in the management of neuropathic pain. Therapeutic Advances in Neurological Disorders, 6(5), 287–297. https://doi. org/10.1177/1756285613496862
• • Barbero, G. F., Liazid, A., Ferreiro-Gonzalez, M., Palma, M., & Barroso, C. G. (2016). Fast separation of capsaicinoids from peppers by reversed phase ultra-performance liquid chromatography: comparation with traditional high-performance liquid chromatography methods. International Journal of Food Properties, 19(5), 984-992. https://doi.org/10.1080/10942912.2015.1050673
• • Benzon, H. T., Rathmell, J. P., Wu, C. L., Turk, D. C., Argoff, C. E., & Hurley, R. W. (2013). Practical Management of Pain: Fifth Edition. Elsevier Inc. https://doi.org/10.1016/C2009-0-64063-0
• • Bononi, M., & Tateo, F. (2012). Determination of capsaicinoids from dried pepper fruits by fast-gas chromatography. Italian Journal of Food Science, 24(1), 49-54.
• • Christo, P. J., & Cauley, B. D. (2009). Chapter 36 - Postherpetic Neuralgia. In: Current Therapy in Pain. Elsevier Inc. pp. 261-267. https:// doi.org/10.1016/B978-1-4160-4836-7.00036-5
• • Ciulu-Costinescu, F., Calina, D., Chirigiu, L., Averis, L. M. E., Rosulescu, E., & Bubulica, M. V. (2015). Identification and quantification of capsaicin from capsicum annuum L. by RP-HPLC. Revista de Chimie, 66(12), 1946–1949.
• • Daood, H. G., Halasz, G., Palotás, G., Palotás, G., Bodai, Z., & Helyes, L. (2015). HPLC determination of capsaicinoids with cross-linked C18 column and buffer-free eluent. Journal of Chromatographic Science, 53(1), 135–143. https://doi.org/10.1093/chromsci/ bmu030
• • Govindarajan, V. S., & Sathyanarayana, M. N. (1991). Capsicumproduction, technology, chemistry, and quality. part v. ımpact on physiology, pharmacology, nutrition, and metabolism; structure, pungency, pain, and desensitization sequences. Critical Reviews in Food Science and Nutrition, 29(6), 435–473. https://doi. org/10.1080/10408399109527536 • Ha, J., Han, K. J., Kim, K. J., & Jeong, S. W. (2008). Gas chromatographic analysis of capsaicin in gochujang. Journal of AOAC International, 91(2), 387–391.
• • Kaale, E., Van Schepdael, A., Roets, E., & Hoogmartens, J. (2002). Determination of capsaicinoids in topical cream by liquid-liquid extraction and liquid chromatography. Journal of Pharmaceutical and Biomedical Analysis, 30(4), 1331–1337. https://doi. org/10.1016/s0731-7085(02)00476-4
• • Kopec, S. E., DeBellis, R. J., & Irwin, R. S. (2002). Chemical analysis of freshly prepared and stored capsaicin solutions: implications for tussigenic challenges. Pulmonary Pharmacology & Therapeutics, 15(6), 529–534. https://doi.org/10.1006/pupt.2002.0394
• • Kuzma, M., Fodor, K., Boros, B., & Perjési, P. (2015). Development and validation of an HPLC-DAD analysis for pharmacopoeial qualification of industrial capsicum extracts. Journal of Chromatographic Science, 53(1), 16–23. https://doi.org/10.1093/chromsci/bmu004
• • Laklouk, M., & Baranidharan, G. (2016). Profile of the capsaicin 8% patch for the management of neuropathic pain associated with postherpetic neuralgia: safety, efficacy, and patient acceptability. Patient Preference and Adherence, 10, 1913–1918. https://doi. org/10.2147/PPA.S76506
• • Lu, M., Ho, C., & Huang, Q. (2017). Extraction, bioavailability, and bioefficacy of capsaicinoids. Journal of Food and Drug Analysis, 25(1), 27–36. https://doi.org/10.1016/j.jfda.2016.10.023
• • Moon, J. Y., Lee, P. B., Kim, Y. C., Lee, S. C., Nahm, F. S., & Choi, E. (2017). Efficacy and safety of 0.625% and 1.25% capsaicin patch in peripheral neuropathic pain: multi-center, randomized, and semi-double blind controlled study. Pain Physician, 20(2), 27–35.
• • Pena-Alvarez, A., Alvarado, L. A., & Vera-Avila, L. E. (2012). Analysis of capsaicin and dıhydrocapsaicin in hot peppers by ultrasound assısted extractıon followed by gas chromatography-mass spectrometry. Instrumentation Science & Technology 40(5), 429–440. https://doi.org/10.1080/10739149.2012.679719
• • Peña-Alvarez, A., Ramírez-Maya, E., & Alvarado-Suárez, L. A. (2009). Analysis of capsaicin and dihydrocapsaicin in peppers and pepper sauces by solid phase microextraction-gas chromatographymass spectrometry. Journal of Chromatography. A, 1216(14), 2843–2847. https://doi.org/10.1016/j.chroma.2008.10.053
• • Surh, Y. J., & Lee, S. S. (1995). Capsaicin, a double-edged sword: toxicity, metabolism, and chemopreventive potential. Life Sciences, 56(22), 1845–1855. https://doi.org/10.1016/0024- 3205(95)00159-4 • Tresh, J. (1876). Isolation of capsaicin. The Pharmaceutical Journal of Transactions, 6, 941–947.
• • Usman, M. G., Rafii, M. Y., Ismail, M. R., Malek, M. A., & Latif, M. A. (2014). Capsaicin and dihydrocapsaicin determination in chili pepper genotypes using ultra-fast liquid chromatography. Molecules, 19(5), 6474–6488. https://doi.org/10.3390/molecules19056474
• • You, Y., Uboh, C. E., Soma, L. R., Guan, F., Taylor, D., Li, X., Liu, Y., & Chen, J. (2013). Validated UHPLC-MS-MS method for rapid analysis of capsaicin and dihydrocapsaicin in equine plasma for doping control. Journal of Analytical Toxicology, 37(2), 122–132. https://doi.org/10.1093/jat/bks098