식품중 불법함유된 발기부전치료제 성분 검출을 위한 동시분석법 연구

Simultaneous Identification/Determination System for Sildenafil, Homosildenafil, Vardenafil and Tadalafil as Adulterants in Foods

  • 발행 : 2003.12.01

초록

본 연구에서는 국내 ${\cdot}$ 외에서 유통되는 건강관련식품 중 성기능 개선 및 효과에 대하여 광고 ${\cdot}$ 판매하고 있는 제품들에 대하여 최근 의약품으로 허가된 발기부전치료제인 sildenafil, vardenafil, tadalafil 및 sildenafil의 유사물질인 homosildenafil을 대상으로 정성과 정량을 위한 동시분석법을 개발하고 유통 제품 중의 함량을 분석하여 함유 실태를 파악하고자 하였다. 네 가지 성분을 확인할 수 있는 TLS와 LC/MS 분석방법을 개발하였으며, LC/PDA를 사용한 동시 정량분석법을 개발하고, 건강보조식품 등 건강관련 식품중 sildenafil 등 4종 물질에 대해 총 35개의 시료를 분석한 결과 sildenafil이 7종에서 0.4 mg/g~360.9 mg/g, homosildenafil이 7종에서 2.2 mg/g~336.0 mg/g, tadalafid이 2종에서 각각 19.2mg/g, 429.3mg/g로 검출되었으며, 본 여구에서 개발한 동시분석법을 유통식품에 적용 가능하였다.

An easily available, simultaneous identification/determination procedure for sildenafil, homosildenafil, tadalafil, vardenafil in adulterated health related foods was established by using a combination of three different analytical methods; thin layer chromatography(TLC), liquied chromatography-mass spectrometry (LC/MS) and high-performance liquied chromatography (HPLC)/photo-diode-array detector. The sample solution for TLC was applied to silica gel 60 $F_{254}$ plates with ethylacetate/acetonitrile/25%ammonia (90:10:5) as a developing solvent. Spots were located under UV radiation at 254 nm and dragendolfs reagent. Mass spectra of the compounds by LC/MS were investigated with electrospray ionization (ESI) interface, under positive ion mode. The HPLC analysis was performed on a column of capcell pack $C_{18}$ (UG120, 4.6${\times}$250mm I.D. 5 ${\mu}$m)with 0.1% sodium 1-hexansulfonate (in 0.1% phosphoric acid)/acetnitrile (73:27) as a mobile phase, and effluent was minitored with a photo-diode-applied to commercial foods, Sildenafil content was inthe range of 0.4mg/g~360.9 mg/g from 7 out of 35 samples. Homosildenafil content was in the range of 2.2 mg/g~336.0 mg/g from 7 out of 35 samples. Tadalafil content was 429.3 mg/g, 9.6 mg/500 mg from 2 out of 35 samples. The procedure described here is available for the screening of sildenafil, homosildenafil, tadalafil, vardenafil.

키워드

참고문헌

  1. Song, I.S., Kim, C.M., Kim, D.B., Park, H.K., Park, K.S., Koo, Y.E., Choi, Y.J., Jang, J.H., Kim, B.Y., Kim, J.J.: The study on the establishment of framework for the regulatory system of functional foods. Korea Food and Drug Administration, Seoul, pp. 137-158 (2002)
  2. 2000 The Study on the trend of New Technology - Functional foods, Korean Intellectual Property Office, Seoul, pp. 201-240 (2000)
  3. Compendium of Asian Patent Medicines. California, California Departrnenet of Health Services, California (1999)
  4. Eiichi Mikami, Tsutomu Ohno and Hiroshi Matsumoto: Simultaneous indentification/determination system for phentolamine and sildenafil as adulterants in soft drinks advertising robornat nutrition, Forensic Science International, 130, 140-146 (2002) https://doi.org/10.1016/S0379-0738(02)00368-7
  5. Shin, M.-H., Hong, M.-K., Kim, W.-S., Lee, Y-J., Jeoung,Y.-C.: Identification of a new analogue of sildenafil added illegally to a functional food marketed for penile erectile dysfunction, Food Additieves & Contaminants, 20(9), 793-796 (2003) https://doi.org/10.1080/0265203031000121455
  6. Daraghmeh, N. et al.: Determination of sildenafil citrate and related substances in the commercial products and tablet dosage form using HPLC, J. of pharmaceutical and Biomedical Analysis, 25, 483-492 (2001) https://doi.org/10.1016/S0731-7085(00)00512-4
  7. Korean Pharmacopoeia ($7^{th}$ ed). Ministry of health and welfare, Seoul (2000)
  8. Takako Moriyasu et al.: Identification system for sildenafil in health foods, Japan Yakugaku zasshi, 121(10), 765-769 (2001) https://doi.org/10.1248/yakushi.121.765
  9. United State Patent: Patent Number 5,250,534,1997
  10. Prickaerts et al.: Effects of two selective phosphodiesterase type 5 inhibiter sidenafil and vardenafil, on object recognition memory and hippocampal cyclic GMP level, Neuroscience, 113(2), 351-361 (2002) https://doi.org/10.1016/S0306-4522(02)00199-9
  11. Noel, N. Kim et al.: Inhibition of cyclic GMP hydrolysis in human corpus cavernosum smooth muscle cells by vardenafil, a novel, selective phosphodiesterase type 5 inhibitor, Life Sciences, 69, 300-304 (2002)
  12. Eardley, I. et al.: Cialis for men with erectile dysfunction, International Journal of Clinical Practics, 56, 300-304 (2002)
  13. Alan M. Laties, Eberhart zrenner: Viagra and ophthalmology. Progress in Retinal and Eye Research, 21, 485-506 (2002) https://doi.org/10.1016/S1350-9462(02)00013-7