Determination of Repertaxin Enantiomeric Purity by HPLC on Chiral Stationary Phase

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• 作者：Yongmei Liu ; Mengya Liao ; Cuiwei Zhang ; Yuli Bai ; Honglian Song…
• 关键词：Column liquid chromatography ; Chiral separation ; Enantiomeric purity ; Repertaxin
• 刊名：Chromatographia
• 出版年：2015
• 出版时间：December 2015
• 年：2015
• 卷：78
• 期：23-24
• 页码：1485-1489
• 全文大小：444 KB
• 参考文献：1.Bertini R, Allegretti M, Bizzarri C, Moriconi A, Locati M, Zampella G, Cervellera MN, Cioccio VD, Cesta MC, Galliera E, Martinez FO, Bitondo RD, Troiani G, Sabbatini V, D’Anniballe G, Anacardio R, Cutrin JC, Cavalieri B, Mainiero F, Strippoli R, Villa P, Girolamo MD, Martin F, Gentile M, Santoni A, Corda D, Poli G, Mantovani A, Ghezzi P, Colotta F (2004) Proc Natl Acad Sci USA 101:11791-1796CrossRef
  2.Garaua A, Bertinib R, Colottab R, Casillib F, Bigini P, Cagnotto A, Mennini T, Ghezzia P, Villa P (2005) Cytokine 30:125-31CrossRef
  3.Bizzarri C, Allegretti M, Di Bitondo R, Cervellera MN, Colotta F, Bertini R (2003) Curr Med Chem Anti Inflamm Anti Allergy Agents 2:67-9CrossRef
  4.Mahida YR, Ceska M, Effenberg F, Kurlak L, Lindley I, Hawkey CJ (1992) Clin Sci 82:273-75CrossRef
  5.Ginestier C, Liu S, Diebel ME, Korkaya H, Luo M, Brown M, Wicinski J, Cabaud O, Charafe-Jauffret E, Birnbaum D, Guan J, Dontu G, Wicha M (2010) J Clin Invest 120:485-97CrossRef
  6.Opfermann P, Derhaschnig U, Felli A, Wenisch J, Santer D, Zuckermann A, Dworschak M, Jilma B, Steinlechner B (2015) Clin Exp Immunol 180:131-42CrossRef
  7.Ha H, Neamati (2014) Mol Pharm 11:2431-441CrossRef
  8.Moriconi A, Bigogno C, Bianchini G, Caligiuri A, Resconi A, Dondio MG, D’Anniballe G, Allegretti M (2011) ACS Med Chem Lett 2:768-73CrossRef
  9.Lacerda L, Pusztai L, Woodwarda WA (2010) Drug Resist Update 13:99-08CrossRef
  10.Bakshi P, Margenthaler E, Laporte V, Crawford F, MullanA M (2008) ACS Chem Biol 12:777-89CrossRef
  11.Casilli F, Bianchini A, Gloaguen I, Biordi L, Alesse E, Festuccia C, Cavalieri B, Strippoli R, Cervellera MN, Di Bitondo R, Ferretti E, Mainiero F, Bizzarri C, Colotta F, Bertini R (2005) Biochem Pharmacol 69:385-94CrossRef
  12.Nair P, Gaga M, Zervas E, Alagha K, Hargreave FE, O’Byrne PM, Stryszak P, Gann L, Sadeh J, Chanez P (2012) Clin Exp Allergy 42:1097-103CrossRef
  13.Allegretti M, Bertini R, Cesta MC, Bizzarri C, Di Bitondo R, Di Cioccio V, Galliera E, Berdini V, Topai A, Zampella G, Russo V, Di Bello N, Nano G, Nicolini L, Locati M, Fantucci P, Florio S, Colotta F (2005) J Med Chem 48:4312-331CrossRef
  14.Tang XH, Yang D, Xie YM, Cao Y, Song H (2009) Chromatographia 70:365-69CrossRef
  15.Xie YM, Luo J, Tang XH, Yang D, Huo XF, Liu A, Hu X, Song X, Song H (2009) Chromatographia 69:1025-029CrossRef
  16.Zuo Z, Hu M, Chen M, Chen X, Yang F, Zeng C, Zhao Y, Zhang Y (2015) Chromatographia 78:579-83CrossRef
  17.Wang Q, Chen X, Zhang C, Liao M, Hu M, Lin S, Xie Y, Yin W, Zhang Y (2015) Chromatographia 78:1395-400CrossRef
  18.Aureli L, Cruciani G, Cesta MC, Anacardio R, De Simone L, Moriconi A (2005) J Med Chem 48:2469-479CrossRef
  19.Sun Q, Olesik SV (2000) J Chromatogr B 745:159-66CrossRef
  20.Ding GS, Liu Y, Cong RZ, Wang JD (2004) Talanta 62:997-003CrossRef
  21.Nageswara Rao R, Narasa Raju A, Nagaraju D (2006) J Pharm Biomed Anal 42:347-53CrossRef
  22.Berthod A, Li W, Armstrong DW (1992) Anal Chem 64:873-79CrossRef
  23.Loun B, Hage DS (1994) Anal Chem 66:3814-822CrossRef
  24.Stringham RW, Blackwell JA (1997) Anal Chem 69:1414-420CrossRef
  
• 作者单位：Yongmei Liu (1)
  Mengya Liao (3)
  Cuiwei Zhang (4)
  Yuli Bai (5)
  Honglian Song (5)
  Yiwen Zhang (1)
  Xin Wang (2)
  
  1. Cancer Center and State Key Laboratory of Biotherapy, Department of Thoracic Oncology, West China Hospital, Sichuan University, Chengdu, 610041, China
  3. Sichuan Academy of Medical Sciences & Sichuan Provincial People’s Hospital, Chengdu, 610072, China
  4. Department of Pathology, The Affiliated Hospital of Luzhou Medical College, Luzhou, 646000, China
  5. The West China School of Pharmacy, Sichuan University, Chengdu, 610041, China
  2. Department of Abdominal Oncology, Cancer Center, West China Hospital, Sichuan University, Chengdu, 610041, China
  
• 刊物类别：Chemistry and Materials Science
• 刊物主题：Chemistry
  Analytical Chemistry
  Organic Chemistry
  Pharmacy
  Biochemistry
  Plant Sciences
  Measurement Science and Instrumentation
  
• 出版者：Vieweg Verlag
• ISSN：1612-1112

文摘

A precise and sensitive LC method for the determination of repertaxin enantiomeric purity has been developed and validated. Baseline separation with a resolution higher than 2.0 was accomplished within 20 min using a Chiralpak AD-H column (250 × 4.6 mm; particle size 5 μm) and n-hexane:2-propanol (90:10 v/v) as mobile phase at a flow rate of 1 mL min?. Eluted analytes were monitored by UV detection at 260 nm. The effects of mobile phase composition, temperature and flow rate on enantiomeric selectivity and on resolution of enantiomers were investigated. Calibration curves were plotted within the concentration range between 0.002 and 1.0 mg mL? (n = 3), and relative standard deviation (RSD) of the inter-batch assay and intra-batch assay was less than 1.27 and 1.16 %. LOD and LOQ for repertaxin were 0.65 and 2.19 μg mL?; those for its enantiomer were 0.70 and 2.34 μg mL?, respectively. The method was evaluated and validated by analysis of bulk samples of repertaxin of different enantiomeric purity. It was demonstrated that the method was accurate, robust, and sensitive, and enabled practical analysis of real samples. Keywords Column liquid chromatography Chiral separation Enantiomeric purity Repertaxin