Nghiên cứu thành phần hóa học và đánh giá tác dụng kháng ung thư của thân lá cây củ dòm Stephania dielsiana Y.C. Wu - 28


5 PHỔ HSQC PL 41 SD06 DMSO HSQC ppm 30 40 50 60 70 80 90 100 110 120 130 140 150 160 170 SD06 1

5. PHỔ HSQC

PL-41

SD06-DMSO-HSQC


ppm 30 40 50 60 70 80 90 100 110 120 130 140 150 160 170 SD06 DMSO HSQC ppm 100 105 110 115 120 125 2

ppm


30


40


50


60


70


80


90


100


110


120


130


140


150


160


170

SD06-DMSO-HSQC


ppm


100


105


110


115


120


125


130


135


140


145


9 8 7 6


5 4 3


ppm


9.0


8.5


8.0


7.5


7.0


6.5


ppm

Phụ lục 3.5. Hợp chất SD5: oxocrebanin

CTPT: C19H13NO5 M = 335

Chất rắn màu vàng cam


MS

1H-NMR (500 MHz, DMSO-d6)

13C-NMR (125 MHz, DMSO-d6)

HMBC HSQC


1. PHỔ MS


Display Report - Selected Window Selected Analysis


Analysis Name:


SD3-1.d Instrument: LC-MSD-Trap-SL


Print Date: 5/20/2020 12:14:09 PM

Method: Sample Name:

Quang_2020.m SD3-1

Operator:

2195410AE0000514

Acq. Date: 5/20/2020 12:11:29 PM

Analysis Info: Column Eclipse XDB-C18, 4.6 x150mm

MSD Trap Report v 4 A4 Opt2 Page 1 of 1 2 PHỔ 1 H NMR 8 758 8 747 8 435 8 417 7 976 7 965 7 593 7 3


MSD Trap Report v 4 (A4-Opt2)

Page 1 of 1

2. PHỔ 1H-NMR


8.758

8.747

8.435

8.417

7.976

7.965

7.593

7.575

7.486

6.463

SD3.1-DMSO-1H


3 936 3 861 3 328 2 507 2 503 2 500 2 496 2 493 Current Data Parameters NAME 11THAO SD3 1 EXPNO 1 4


3 936 3 861 3 328 2 507 2 503 2 500 2 496 2 493 Current Data Parameters NAME 11THAO SD3 1 EXPNO 1 5

3.936

3.861

3.328

2.507

2.503

2.500

2.496

2.493

Current Data Parameters NAME 11THAO_SD3.1

EXPNO 1

PROCNO 1

F2 - Acquisition Parameters Date_ 20200301

Time 17.26

INSTRUM spect PROBHD 5 mm PABBO BB/ PULPROG zg30

TD 65536

SOLVENT DMSO

NS 32

DS 2

SWH 10000.000 Hz

FIDRES 0.152588 Hz

AQ 3.2767999 sec

RG 127.68

DW 50.000 usec

DE 6.50 usec

TE 303.4 K

D1 1.00000000 sec

TD0 1

======== CHANNEL f1 ======== SFO1 500.1920889 MHz NUC1 1H

P1 10.20 usec

PLW1 22.00000000 W

SI SF WDW

SSB


0

65536

500.1890053 MHz

EM

LB


0.30 Hz

GB

0


PC


1.00

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F2 - Processing parameters


1.00

1.00

1.03

1.08

1.07

2.01

3.14

3.14

13 12 11 10 9 8 7 6 5 4 3 2 1 0


8 758 8 747 8 435 8 417 7 976 7 965 7 593 7 575 7 486 6 463 3 936 3 861 SD3 1 DMSO 1H 1 ppm 1 00 1 10

8.758

8.747

8.435

8.417

7.976

7.965

7.593

7.575

7.486

6.463

3.936

3.861

SD3.1-DMSO-1H

-1 ppm



1 00 1 00 1 03 1 08 1 07 2 01 3 14 3 14 9 0 8 5 8 0 7 5 7 0 6 5 6 0 5 5 5 0 4 5 4 0 ppm 8 758 8 747 19


1.00

1.00

1.03

1.08

1.07

2.01

3.14

3.14

9.0 8.5

8.0

7.5

7.0

6.5

6.0

5.5

5.0

4.5

4.0

ppm

8 758 8 747 8 435 8 417 7 976 7 965 7 593 7 575 7 486 SD3 1 DMSO 1H 1 00 1 00 1 03 1 08 1 07 8 9 8 35

8.758

8.747

8.435

8.417

7.976

7.965

7.593

7.575

7.486

SD3.1-DMSO-1H



1 00 1 00 1 03 1 08 1 07 8 9 8 8 8 7 8 6 8 5 8 4 8 3 8 2 8 1 8 0 7 9 7 8 7 7 7 6 7 5 ppm 3 PHỔ 13 43


1.00

1.00

1.03

1.08

1.07

8.9 8.8

8.7

8.6

8.5

8.4

8.3

8.2

8.1

8.0

7.9

7.8

7.7

7.6

7.5

ppm


3. PHỔ 13C-NMR


180.78

153.28

151.69

150.02

145.63

144.19

135.06

125.97

125.36

123.84

123.51

121.34

118.13

106.90

102.89

102.15

60.58

56.14

40.00

39.83

39.67

39.50

39.33

39.17

39.00

SD3.1-DMSO-C13CPD



Current Data Parameters NAME 11THAO_SD3.1

EXPNO 2 PROCNO 1 F2 Acquisition Parameters Date 20200301 Time 18 04 INSTRUM spect PROBHD 5 mm PABBO 55

EXPNO 2

PROCNO 1

F2 - Acquisition Parameters Date_ 20200301

Time 18.04

INSTRUM spect PROBHD 5 mm PABBO BB/

PULPROG zgpg30

TD 65536

SOLVENT DMSO

NS 4096

DS 4

SWH 31250.000 Hz

FIDRES 0.476837 Hz

AQ 1.0485760 sec

RG 198.57

DW 16.000 usec

DE 6.50 usec

TE 304.2 K

D1 2.00000000 sec

D11 0.03000000 sec

TD0 1

======== CHANNEL f1 ======== SFO1 125.7864591 MHz NUC1 13C

P1 10.00 usec

PLW1 88.00000000 W

======== CHANNEL f2 ======== SFO2 500.1910008 MHz NUC2 1H

CPDPRG[2 waltz16

PCPD2 80.00 usec

PLW2 22.00000000 W

PLW12 0.35764000 W

PLW13 0.17989001 W

SI SF WDW

SSB


0

32768

125.7726241 MHz

EM

LB


1.00 Hz

GB

0


PC


1.40

F2 - Processing parameters


220 200 180 160 140 120 100 80 60 40 20 0 ppm



180 155 153 28 170 150 151 69 150 02 160 145 145 63 150 SD3 1 DMSO C13CPD 140 144 19 140 130 135 56

180 155 153 28 170 150 151 69 150 02 160 145 145 63 150 SD3 1 DMSO C13CPD 140 144 19 140 130 135 57

180

155

153.28


170

150

151.69


150.02


160

145

145.63

150

SD3.1-DMSO-C13CPD

140

144.19


140

130

135

130

135.06


120

110

125

125.97

125.36

123.84

123.51


100

120

121.34


90

80

115

118.13


70

110

105

106.90


60

102.89

ppm

ppm

102.15

180.78


153.28

151.69

SD3.1-DMSO-C13CPD

150.02


145.63

144.19


135.06


125.97

PL-45

125.36

123.84

123.51

121.34

118.13


106.90

102.89

102.15


60.58

56.14


SD3 1 DMSO HMBC ppm 30 40 50 60 70 80 90 100 110 120 130 140 150 160 170 180 190 SD3 1 DMSO HMBC 88

SD3.1-DMSO-HMBC


ppm


30


40


50


60


70


80


90


100


110


120


130


140


150


160


170


180


190

SD3.1-DMSO-HMBC


ppm 95 100 105 110 115 120 125 130 135 140 145 150 155 160 4 PHỔ HMBC PL 46 8 7 6 5 4 3 ppm 8 5 8 89

ppm


95


100


105


110


115


120


125


130


135


140


145


150


155


160


4. PHỔ HMBC

PL-46

8 7 6 5 4 3

ppm

8.5

8.0

7.5

7.0

6.5

6.0

5.5

5.0

4.5

4.0

ppm


SD3.1-DMSO-HMBC


ppm 100 105 110 115 5 PHỔ HSQC 120 125 130 135 140 145 150 SD3 1 DMSO HSQC ppm 30 40 50 60 70 80 90

ppm 100


105


110


115


5. PHỔ HSQC

120


125


130


135


140


145


150

SD3.1-DMSO-HSQC


ppm


30


40


50


60


70


80


90


100


110


120


130


140



8.8 8.6


8.4


8.2


8.0


7.8


7.6


7.4


7.2


7.0


6.8


6.6

155

PL 47 ppm 9 8 7 6 5 4 3 2 150 1 ppm SD3 1 DMSO HSQC ppm 100 105 110 115 120 125 130 135 140 145 PL 91

PL-47

ppm


9 8 7


6 5 4 3 2

150

1 ppm


SD3 1 DMSO HSQC ppm 100 105 110 115 120 125 130 135 140 145 PL 48 9 0 8 5 8 0 7 5 7 0 6 5 ppm 92

SD3.1-DMSO-HSQC


ppm 100


105


110


115


120


125


130


135


140


145


PL-48

9.0 8.5

8.0

7.5

7.0

6.5

ppm

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