采用三聚氯氰为活化剂分别合成了牛血清白蛋白（BSA）、人血清白蛋白（HSA）和β-环糊精手性固定相，研究了温度在色氨酸,华法令，酮基布洛芬和丹酰化苏氨酸手性拆分中的影响。结果表明，在蛋白手性固定相上对映体间的熵变对色氨酸,华法令和酮基布洛芬的拆分有很大的影响，而丹酰化苏氨酸对映体在β-环糊精手性固定相上的拆分为典型的焓控过程，与蛋白柱有着不同的热力学特性。由于键合方式不同，色氨酸在我们合成的BSA手性固定相上的最佳分离温度为35℃左右，而不是文献报道的以戊二醛为活化剂的24℃。
The effect of column temperature on enantiomeric resolution s oftryptophan, warfarin and ketoprofen was investigated on bovine and human serum albumin (BSA and HSA) stationary phases, which were synthesized with s-triazine as the activator. It was observed that the e ntropy change made a great contribution to the separation of those enantiomers o n albumin chiral stationary phases. The column temperature for the maximal resol ution of tryptophan on the BSA stationary phase prepared by this method was abou t 35 ℃, which was not 24 ℃ as reported for the BSA stationary phase sy n thesized with glutaric dialdehyde as the activator. This results may come from the different conformation of the immobilized BSA and HSA due to the different c oupling methods used. On the other hand, it was indicated that the resolution of enantiomers on β -CD chiral stationary phase was mainly contributed from the change of enthalp y, which means the resolution of chiral solutes on albumin and β-CD statio nary phases has different thermodynamic behaviors.
参考文献
| [1] | Erlandsson P, Marle I, Hansson L, et al. J Am Chem Soc, 1990,1 12:4 573-4 574 |
| [2] | Armstrong D W, Ward T J, Armstrong R D, et al. Science, 1985,232:1 132- 1 135 |
| [3] | Peters T J. Advances in protein chemistry, Vol.37. New York:Academic Pre ss, 1985.161-215 |
| [4] | He X M, Carter D C. Nature, 1992,358:209-214 |
| [5] | Stewart K K, Doherty R F. Proc Natl Acad Sci USA,1973,70:2 850 |
| [6] | Domenici E, Bertucci C, Salvadori P, et al. Chromtographia, 1990,29:17 0-176 |
| [7] | Zhang Q, Zou H F, Wang H L, et al. J Chromatogr A, 2000, 866:173-181 |
| [8] | Zhang Q, Zou H F, Chen X M, et al. Chirality, 2000,12:714-719 |
| [9] | HUANG Tian-bao，WU Bang-gui，LONG Yuan-de. Chinese Journal of Analytical Chemistry， 1991，19 (11），1 257-1 260黄天宝,吴邦贵,龙远德. 分析化学， 1991，19 (11）：1 257-1 260 |
| [10] | ZHANG Qiang，ZOU Han-fa，WANG Hai-lin,et al. CN 99113091.X, 1999张 强,邹汉法,汪海林,等. 中国专利：99113091.X， 1999 |
| [11] | Koppenhoefer B, Bayer E. Chromatographia, 1984, 19:123-130 |
| [12] | Stringham R W, Blackwell J A. Anal Chem, 1997, 69:1 414-1 420 |
| [13] | Gilpin R K, Ehtesham S E, Gregory R B. Anal Chem, 1991, 63:2 825-2 828 |
| [14] | Yang J, Hage D S. J Chromatogr, 1993, 645:241-250 |
| [15] | Zhang Q, Zou H F, Wang H L, et al. Chromatographia, submitted for publ ication |
- 下载量()
- 访问量()
- 您的评分：
-
10%
-
20%
-
30%
-
40%
-
50%