Analytical Science and Technology (분석과학)

The Korean Society of Analytical Sciences (한국분석과학회)
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Qunatitative analysis of liquiritin and glycyrrhizin in glycyrrhizae radix by HPLC-MS/MS

HPLC-MS/MS에 의한 감초의 liquiritin과 glycyrrhizin의 분석

  • Yu, Young-Beob (Dept. of Herbal Pharmaceutical Development, Korea Institute of Oriental Medicine) ;
  • Kim, Mi-Jung (Dept. of Herbal Pharmaceutical Development, Korea Institute of Oriental Medicine) ;
  • Huang, Dae Sun (Dept. of Herbal Pharmaceutical Development, Korea Institute of Oriental Medicine) ;
  • Ha, Hye-Kyeong (Dept. of Herbal Pharmaceutical Development, Korea Institute of Oriental Medicine) ;
  • Ma, Jin-Yeul (Dept. of Herbal Pharmaceutical Development, Korea Institute of Oriental Medicine) ;
  • Shin, Hyeun-Kyoo (Dept. of Herbal Pharmaceutical Development, Korea Institute of Oriental Medicine)
  • 유영법 (한국한의학연구원 한약제제연구부) ;
  • 김미정 (한국한의학연구원 한약제제연구부) ;
  • 황대선 (한국한의학연구원 한약제제연구부) ;
  • 하혜경 (한국한의학연구원 한약제제연구부) ;
  • 마진열 (한국한의학연구원 한약제제연구부) ;
  • 신현규 (한국한의학연구원 한약제제연구부)
  • Received : 2007.05.16
  • Accepted : 2007.08.03
  • Published : 2007.08.25
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Abstract

Licorice, Glycyrrhizae Radix is widely used as a herbal medicines and a dietary supplements in East Asia. We employed high performance liquid chromatography electrospray ionization tandem mass spectrometry to determine liquiritin and glycyrrhizin in the Glycyrrhizae Radix. Liquiritin and glycyrrhizin in Glycyrrhizae Radix were ionized by positive ion pneumatically assisted electrospray and detected by HPLC-MS/MS in the multiple-reaction monitoring (MRM) mode using precursor ${\rightarrow}$ product ion combinations at m/z $436.2{\rightarrow}257.0$ and $823.4{\rightarrow}453.4$, respectively. The assay had a calibration range from 10 to 3,000 ng/mL. The limits of detection (LOD) of the liquiritin and glycyrrhizin were 0.4 ng/mL and 0.01 ng/mL, respectively. The reproducibility and repeatability (relative standard deviation) at different analyte concentrations varied from 103 to 113 % and 0.95 to 1.8 %, respectively. According to the above results, HPLC-MS/MS method permits assignment of tentative structures such as liquiritin and glycyrrhizin in the Glycyrrhizae Radix.

한약과 기능성식품으로 널리 활용되는 감초의 지표물질인 glycyrrhizin과 liquiritin을 HPLC-MS/MS 로 정성, 정량분석을 실시하였다. 두 가지 지표성분 모두 positive ion mode에서 검출이 가능하였고, precursor ion과 product ion을 조합한 multiple-reaction monitoring (MRM) mode에서 liquiritin은 m/z $436.2{\rightarrow}257.0$로 관찰되었고, glycyrrhizin은 m/z $823.4{\rightarrow}453.4$ 로 각각 검지되었다. 감초 물 추출물을 분무건조기로 건조한 분말에서 glycyrrhizin의 경우 5.8%, liquiritin의 경우 2.3% 각각 함유되어 있었다. 회수율은 103-113%였고, 일간, 일내 정밀도 실험에서 상대표준편차는 0.95-1.8% 였다. 본 실험 조건에서 liquiritin과 glycyrrhizin의 검출한계는 각각 0.4 ng/mL과 0.01 ng/mL 이었다.

Keywords

References

  1. 식품의약품안전청, '대한약전', 제8개정, 식품의약품 안전청고시 제2002-15호, 서울, 대한민국, 2002
  2. 식품의약품안전청, '대한약전외한약(생약)규격집', 서울, 식품의약품안전청고시 제2004-17호, 대한민국, 2004
  3. 조선민주주의인민공화국 보건부 약전위원회, '조선민주주의인민공화국 약전', 제5판, 평양 의과학출판사, 평양, 조선인민민주주의공화국, 1996
  4. 일본약국방해설서 편집위원회, '일본약국방해설서', 제14개정, 광천서림, 동경, 일본, 2001
  5. 국가약전위원회, '중화인민공화국약전', 2000년판 1부, 화학공업출판사, 북경, 중화인민공화국, 2000
  6. WHO, 'WHO monographs on selected medicinal plants', 1-20, Geneva, Swiss, 1998
  7. B. A. Olsen, B. C. Castle, D. P. Myers, Trend Anal. Chem., 25, 796-805 (2006) https://doi.org/10.1016/j.trac.2006.06.005
  8. M. L. Gross and R. M. Caprioli, 'The encyclopedia of Mass Spectrometry', 1st ed., Vol. 6, 401, Elsevier, Amsterdam, Netherlands, 2007
  9. J. F. Mora, G. J. Van Berkel, C. G. Enke, R. B. Cole, M. Martinez-Sanchez, J. B. and Fenn., J. Mass. Spectrom. 35(8), 939-952 (2000) https://doi.org/10.1002/1096-9888(200008)35:8<939::AID-JMS36>3.0.CO;2-V
  10. A. P. Bruins, J. chromatogr. A, 794, 345-357 (1998) https://doi.org/10.1016/S0021-9673(97)01110-2
  11. J. H., Park, Pharmacon. 21, 30-38 (1991)
  12. M. Herderich, E. Richling, R. Roscher, C. Schneider, W. Schwab W, H. U. Humpf and P. Schreier, Chromatographia, 45, 127-132 (1997) https://doi.org/10.1007/BF02505549
  13. Y. B. Yu, Y. S. Yoon and G. H. Cho, J. Korean Oriental Med., 25, 45-54 (2004)
  14. Y. B. Yu, S. H. Kim and Y. S. Yoon, J. Toxicol. Pub. Health, 21, 255-261 (2005)
  15. B. C. Liau, S. S. Hsiao, M. R. Lee, T. T. Jong and S. T. Chiang, J. Pharm.Biomed. Anal. 43, 1174-1178 (2007) https://doi.org/10.1016/j.jpba.2006.10.002
  16. B. FU, H. Li, X. Wang, F.S.C. Lee and S. Cui, J. Agric. Food Chem., 53, 7408-7414 (2005) https://doi.org/10.1021/jf051258h
  17. L. Li, S. Liang, F. Du and C. Li, J. Am. Soc. Mass Spectrom., 18, 778-782 (2007) https://doi.org/10.1016/j.jasms.2006.12.011
  18. Z. J. Lin, S. X. Qiu, A. Wufer and L. Shum, J. Chromatogr. B, 814, 201-207 (2005) https://doi.org/10.1016/j.jchromb.2004.10.026
  19. S. Shibata, K. Takahashi, S. Yano, M. Harada, H. Saito, Y. Tamura, A. Kumagai, K. Hirabayashi, M. Yamamoto and N. Nagata, Chem. Pharm. Bull., 35, 1910- 1918 (1987) https://doi.org/10.1248/cpb.35.1910
  20. T. Nakanishi, A. Inada, K. Kambayashi and K. Yoneda, Phytochemistry, 24, 339-341 (1985) https://doi.org/10.1016/S0031-9422(00)83548-7
  21. R. Takeda, I. Miyamori, R. Soma, T. Matsubara and M. Ikeda, J. Steroid Biochem., 27, 845-849 (1987) https://doi.org/10.1016/0022-4731(87)90158-0
  22. Y. Sato, JX. He, H. Nagai, T. Tani and T. Akao, Biol. Pharm. Bull., 30, 145-149, (2007) https://doi.org/10.1248/bpb.30.145