黄花石蒜中化学成分的研究(5)

提取分离过程如图3-4所示：

图3-4黄花石蒜的提取分离过程
Figure 3-4 The Extraction and Isolation of Lycoris aurea Herb.
4. 结果和讨论
4.1 分离所得化合物的结构鉴定
Adenosine (1) ，无色针状结晶，易溶于二甲亚砜，微溶于水和甲醇。1H-NMR ( 400 MHz, d6-DMSO, ppm): 8.35(1H, s), 8.15(1H, s), 7.32(2H, s,NH2 ), 5.84(1H, d, J =6.1), 5.42( 2H, d, J =6.0), 5.16 ( 1H, d, J =4.0 ), 4.62 ( 1H, dd, J =5.6, 11.0 ), 4.16( 1H, m ), 3.97 ( 1H, d, J =10.2 )。13C-NMR ( 100 MHz, d6-DMSO, ppm ) : 156.1, 152.3, 129.0, 139.9, 119.3, 87.9, 85.8, 73.4, 70.6, 61.6。与文献[15]报道的数据一致。化合物1结构，如图4-1-1所示：

图4-1-1化合物1的结构
Figure 4-1-1 The structure of compound 1
2-Deoxyadenosine (2)，白色粉末，溶于甲醇。1H-NMR (400 MHz, CD3OD, ppm): 8.36(1H, s), 8.21(1H, s), 6.47(1H, dd, J =6.0, 8.2), 4.62(1H, m), 4.11( 1H, dd, J =3.2, 5.6 ), 3.89( 1H, dd, J =3.0,12.6 ), 3.87(1H, dd, J =3.2, 12.2), 2.85(1H, ddd, J =5.7, 8.2, 13.5), 2.45(1H, ddd, J =2.5,5.8,13.3)。13C-NMR (100 MHz, CD3OD, ppm): 157.8,153.8,150.3,141.8,119.7, 90.2, 87.4,73.3,63.9, 41.9。LC-MS(pos.): 274[M+Na]+, 136.1[M+2H-C5H9O3]+与文献[16]报道的数据一致。化合物2结构，如图4-1-2所示：

图4-1-2化合物2的结构
Figure 4-1-2 The structure of compound 2
Guanosine (3)，白色粉末，易溶于二甲亚砜，微溶于水和甲醇。1H-NMR ( 400 MHz, d6-DMSO, ppm):7.94(1H,s), 5.70(1H, d, J =6.0), 4.40( 1H, T, J = 5.4), 4.09( 1H, t, J =3.6), 3.88(1H,dd, J =3.6, 7.2), 3.61(1H, dd, J =3.8, 12.0), 3.52(1H, dd, J =4.1, 12.0)。13C-NMR (100 MHz, d6-DMSO, ppm): 156.9,153.7,151.5,135.8, 116.8, 86.5, 85.3, 73.8, 70.5, 61.4。ESI-MS (pos.): 284[M+1]+ ; ESI-MS(neg.): 282[M-1]-。与文献[16]报道的数据一致。化合物3结构，如图4-1-3所示：

图4-1-3化合物3的结构
Figure 4-1-3 The structure of compound 3

2’-Deoxyguanosine hydrate (4)，白色粉末，易溶于二甲亚砜，微溶于水和甲醇。1H-NMR ( 400 MHz, d6-DMSO, ppm):7.95(1H,s), 10,7(1H, s), 6.50(1H, s), 5.10(1H, s), 6.14(1H,m),
3.55(1H,m), 3.83(1H, m), 4.36(1H, m), 2.53(1H, m), 2.22(1H, m), 5.31(1H,m)。13C-NMR (100 MHz, d6-DMSO, ppm): 156.7, 153.7, 150,9, 135.3, 116.6, 87.6, 82.6,70.7, 61.7, 39.5。与文献[17]报道的数据一致。化合物4结构，如图4-1-4所示：

图4-1-4化合物4的结构
Figure 4-1-4 The structure of compound 4

Thymidine (5)，白色粉末，溶于水和甲醇。1H-NMR ( 400 MHz, D2O, ppm):7.72(1H, d, J =1.3), 6.34(1H, t, J =6.7), 4.54(1H, dd, J =4.6, 9.7), 4.10(1H,dd, J =4.0, 8.5), 3.91(1H, dd, J =3.6, 12.6), 3.83(1H, dd, J =5.0,12.6), 2.43(2H, m), 1.95( 3H, d, J =1.2,CH3)。13C-NMR (100 MHz, D2O, ppm): 169,154.3,140.1,114.0,89.2,87.7,73.1,63.9,41.2,14.2。LC-MS(pos.)
: 265[M+Na]+, 529[2M+COOH]+; LC-MS(neg.): 241[M-1]-, 483.2[2M-1]-。与文献[18]报道的数据一致。化合物5结构，如图4-1-5所示：

图4-1-5化合物5的结构
Figure 4-1-5 The structure of compound 5

Phenylalanine (6)，白色粉末，易溶于二甲亚砜，微溶于水和甲醇。1H-NMR ( 100 MHz, TFA, ppm):7.45(2H,dd), 7.3(2H,d), 7.45(1H,dd), 3.37(1H,dd), 3.64(1H,dd), 7.33(3H), 4.68
(1H,t)。13C-NMR (100 MHz, d6-DMSO,ppm):130.7,129.5,131.1,145,37.5,57.3,175.0。与文献[19]报道的数据一致。化合物6结构，如图4-1-6所示：

图4-1-6化合物6的结构
Figure 4-1-6 The structure of compound 6

Tryptophan (7)，白色粉末，易溶于二甲亚砜，微溶于水和甲醇。1H-NMR ( 400 MHz, d6-DMSO, ppm):7.6 (1H, d, J = 7.7), 7.36 (1H, d, J =8.0), 7.27(1H, s), 7.06(1H, dd, J = 7.3, 7.6), 6.97( 1H, dd, J =7.5, 7.2), 3.59(1H,brs), 3.35( 1H, d, J =13.3), 3.05(1H, m)。13C-NMR (100 MHz, d6-DMSO, ppm): 171.5, 136.3, 127.3, 124.2, 121.0, 118.5, 118.4, 111.4, 109.3, 54.7, 22.3。与文献[20]报道的数据一致。化合物7结构，如图4-1-7所示：黄花石蒜中化学成分的研究(5):http://www.751com.cn/huaxue/lunwen_598.html