Page 101 - 《中国药房》2022年5期
P. 101
(C-11),122.9(C-12),144.1(C-13),42.1(C-14),28.3 C-1~C-5(104.7,75.4,75.2,69.9,66.3),Rha C-1~C-6
(C-15),23.4(C-16),47.0(C-17),41.7(C-18),46.2 (101.3,72.0,81.1,72.8,69.8,18.2),Rib C-1~C-5
(C-19),30.7(C-20),34.0(C-21),32.5(C-22),28.8 (104.7,72.8,70.3,68.9,65.3),Glc C-1~C-6(95.7,74.1,
[26]
(C-23),16.5(C-24),15.6(C-25),17.5(C-26),26.1 79.3,71.1,78.9,62.2)。对比参考文献波谱数据 ,鉴定
(C-27),176.5(C-28),33.1(C-29),23.7(C-30),GlcⅠ 该化合物为clemastanoside D。
C-1~C-6(95.7,73.8,78.8,70.8,78.1,69.2),GlcⅡ C-1~ 化 合 物 11:白 色 无 定 形 粉 末 。 ESI-MS 显 示 m/z
C-6(104.9,75.3,76.5,78.2,77.2,61.3),Rha C-1~C-6 951 [M+Na] ,综合其1D-NMR数据分析,推测其分子式
+
(102.7,72.6,72.8,74.0,70.3,18.5)。对比参考文献波谱 为 C47H76O18。 H-NMR(500 MHz,C5D5N)显示 6 个甲基
1
[25]
数据 ,鉴定该化合物为cussonside B。 质子信号:δH 0.86,0.87,0.94,1.01,1.15,1.18(each 3H,s,
化 合 物 9:白 色 无 定 形 粉 末 。 ESI-MS 显 示 m/z CH3 );3 个糖端基质子信号:δ H 6.31(1H,J=8.1 Hz,
-
941 [M-H] ,综合其1D-NMR数据分析,推测其分子式 28-O-Glc H-1),5.16(1H,d,J=7.6 Hz,3-O-Glc H-1)和
为 C48H78O18。 H-NMR(500 MHz,C5D5N)显示 6 个甲基 5.15(1H,d,J=5.8 Hz,Ara H-1);苷元部分特征质子信
1
质子信号:δH 0.84,0.86,0.99,1.04,1.12,1.15(each 3H,s, 号:δ H 3.18(1H,dd,J=4.1、13.7 Hz,H-18),5.42(1H,br s,
CH3 );3 个糖端基质子信号:δ H 5.84(1H,br s,Rha H-1), H-12)。 C-NMR(125 MHz,C5D5N)中δ C:38.8(C-1),
13
6.22(1H,d,J=8.1 Hz,GlcⅠH -1)和 4.97(1H,d,J=7.8 26.1(C-2),82.1(C-3),43.5(C-4),47.0(C-5),18.3(C-6),
Hz,GlcⅡH -1);Rha的甲基质子信号:δH 1.67(3H,d,J= 32.6(C-7),40.0(C-8),48.2(C-9),36.9(C-10),23.4
6.2 Hz);苷元部分特征质子信号:δ H 3.16(1H,dd,J= (C-11),122.9(C-12),144.2(C-13),42.2(C-14),28.3
4.1、13.7 Hz,H-18),5.41(1H,br s,H-12)。 C-NMR (C-15),23.4(C-16),47.0(C-17),41.8(C-18),46.2
13
(125 MHz,C5D5N)中 δ C:38.8(C-1),27.7(C-2),73.4 (C-19),30.8(C-20),34.0(C-21),32.5(C-22),64.9
(C-3),42.9(C-4),48.1(C-5),18.5(C-6),32.5(C-7),39.9 (C-23),13.5(C-24),16.2(C-25),17.6(C-26),26.1
(C-8),48.5(C-9),37.2(C-10),23.8(C-11),122.9 (C-27),176.5(C-28),33.1(C-29),23.7(C-30),Ara
(C-12),144.1(C-13),42.1(C-14),28.3(C-15),23.3 C-1~C-5(104.0,81.4,73.7,68.4,65.1),3-O-Glc C-1~
(C-16),47.0(C-17),41.7(C-18),46.2(C-19),30.7 C-6(106.0,76.3,78.4,71.4,78.3,62.6),28-O-Glc C-1~
(C-20),33.9(C-21),32.5(C-22),67.8(C-23),13.1 C-6(95.8,74.2,79.0,71.2,79.4,62.3)。对比参考文献波
(C-24),161.0(C-25),17.6(C-26),26.0(C-27),176.5 谱数据 ,鉴定该化合物为 3β-O-β-D-吡喃葡萄糖-(1→
[27]
(C-28),33.1(C-29),23.6(C-30),GlcⅠ C-1~C-6(95.6, 2)-α-L-吡喃阿拉伯糖-常春藤皂苷元-28-O-β-D-吡喃葡
73.8,78.7,70.8,78.0,69.2),Glc Ⅱ C-1~C-6(104.9, 萄糖酯苷。
75.3,76.5,78.2,77.1,61.3),Rha C-1~C-6(102.7,72.6, 化 合 物 12:白 色 无 定 形 粉 末 。 ESI-MS 显 示 m/z
+
72.7,74.0,70.3,18.6)。对比参考文献波谱数据 ,鉴定 1 081 [M+Na] ,综合其 1D-NMR 数据分析,推测其分子
[22]
该化合物为白头翁皂苷C。 式为 C53H86O21。 H-NMR(500 MHz,C5D5N)显示 7 个甲
1
化 合 物 10:白 色 无 定 形 粉 末 。 ESI-MS 显 示 m/z 基质子信号:δ H 0.85,0.85,0.86,0.92,1.05,1.20,1.22
1 067 [M+Na] ,综合其 1D-NMR 数据分析,推测其分子 (each 3H,s,CH3 );4 个糖端基质子信号:δ H 4.73(1H,d,
+
1
式为 C52H84O21。 H-NMR(500 MHz,C5D5N)显示 6 个甲 J=6.9 Hz,Ara H-1),5.81(1H,br s,Rha H-1),6.19(1H,
基质子信号:δ H 0.86,0.87,0.94,1.10,1.12,1.18(each d,J=8.0 Hz,GlcⅠ H-1)和4.92(1H,d,J=7.8 Hz,GlcⅡ
3H,s,CH3 );4 个糖端基质子信号:δ H 6.32(1H,br s,Rha H-1);Rha 的甲基质子信号:δ H 1.68(3H,d,J=6.1 Hz);
H-1),6.31(1H,d,J=8.2 Hz,Glc H-1),5.95(1H,d,J= 苷元部分特征质子信号:δ H 3.11(1H,m,H-3),3.30(1H,
4.5 Hz,Rib H-1)和 5.04(1H,d,J=6.8 Hz,AraH-1);Rha dd,J=3.1、11.2 Hz,H-18),5.38(1H,br s,H-12)。
的甲基质子信号:δH 1.53(3H,d,J=6.2 Hz);苷元部分特 13 C-NMR(125 MHz,C5D5N)中δ C:38.7(C-1),26.4(C-2),
征质子信号:δH 3.17(1H,dd,J=4.1、13.7 Hz,H-18),5.40 88.6(C-3),39.4(C-4),55.7(C-5),18.4(C-6),33.0(C-7),
(1H,br s,H-12)。 C-NMR(125 MHz,C5D5N)中δ C:39.1 39.8(C-8),48.0(C-9),36.9(C-10),23.7(C-11),122.8
13
(C-1),26.2(C-2),81.2(C-3),43.6(C-4),47.7(C-5),18.2 (C-12),144.0(C-13),42.0(C-14),28.1(C-15),23.2
(C-6),32.8(C-7),39.8(C-8),48.2(C-9),36.8(C-10), (C-16),46.9(C-17),41.5(C-18),46.1(C-19),30.6
23.7(C-11),122.9(C-12),144.0(C-13),42.1(C-14),28.3 (C-20),33.9(C-21),32.4(C-22),28.1(C-23),16.8
(C-15),23.6(C-16),46.6(C-17),41.7(C-18),46.2 (C-24),15.5(C-25),17.4(C-26),26.0(C-27),176.4
(C-19),30.8(C-20),34.0(C-21),32.5(C-22),63.9 (C-28),33.0(C-29),23.6(C-30),Ara C-1~C-5(107.4,
(C-23),14.2(C-24),16.2(C-25),17.5(C-26),26.1 72.8,74.5,69.4,66.6),GlcⅠ C-1~C-6(95.5,73.7,78.6,
(C-27),176.4(C-28),33.2(C-29),23.7(C-30),Ara 70.7,77.9,69.0),Glc Ⅱ C-1~C-6(104.7,75.2,76.4,
中国药房 2022年第33卷第5期 China Pharmacy 2022 Vol. 33 No. 5 ·607 ·