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Cell culture and AMPK assay by Western blot analysisHPLC analysis of active compounds and myristicin under different extraction conditionsExtraction and isolation of active compounds on AMPK from Myristica fragransProcessing procedures for reducing myristicin contents from extracts of Myristica fragransAnimal experiments

Trang 1

Le Thi Van Thu Advisor: Prof Oh Won-Keun Ph.D Department of Pharmacy,

Graduate School of Chosun University

October, 2009

Thesis for Master Degree

Trang 2

Metabolic syndrome

WHO definition of the metabolic syndrome, 1999

Glucose intolerance or diabetes mellitus and/or insulin resistance together with two or more of the other components listed below:

 Impaired glucose regulation or diabetes;

 Insulin resistance

 Raised arterial pressure ≥ 140/90 mmHg;

 Raised plasma triglycerides and/or low HDL-cholesterol

 Central obesity

Trang 3

 Consequences of the syndrome

 Cardiovascular disease, hypertension and chronic renal disease

 Diabetes and obesity

Trang 4

 AMP activated protein kinase:

a target for total metabolic control

Structure and regulation of AMPK

Trang 5

 Acyl CoA carboxylase and fat metabolism

Trang 6

Uses: spice, cosmetic,

drugs.

Part used: seed

Trang 7

 Cell culture and AMPK assay by Western blot analysis

 HPLC analysis of active compounds and myristicin under different extraction conditions

 Extraction and isolation of active compounds on AMPK

from Myristica fragrans

 Processing procedures for reducing myristicin contents

from extracts of Myristica fragrans

 Animal experiments

Trang 8

Mob Phase: EtOH:H2O

60% EtOH 80% EtOH 90% EtOH 100% EtOH Aceton

OP-CC (6 × 60 cm), Silica gel (63 - 200 µm)

Sol System: n-Hexan: Aceton (6:1 - 0:1)

Compound 6 (12 mg)

Compound 7 (8.5 mg)

Compound 1 (370 mg)

Compound 2 (28.9 mg) Compound 3 (12.7 mg) Compound 4 (6.7 mg) Compound 5 (7.8 mg)

OP-CC (5 × 60 cm)

RP ODS-A (12 nm) MeOH: H2O

Trang 9

Structure determination of tetrahydrofuran type-lignans from

Myristica fragrans

13C-NMR

Compound 1

Trang 10

Structure determination of tetrahydrofuran type-lignans from

Myristica fragrans

13C-NMR

Compound 2

Trang 11

Structure determination of tetrahydrofuran type-lignans from

Myristica fragrans

13C-NMR

Compound 3

Trang 12

Structure determination of tetrahydrofuran type-lignans from

Myristica fragrans

13C-NMR

Compound 4

Trang 13

Structure determination of tetrahydrofuran type-lignans from

Myristica fragrans

13C-NMR

Compound 5

Trang 14

Structure determination of tetrahydrofuran type-lignans from

Myristica fragrans

13C-NMR

Compound 6

Trang 15

Structure determination of tetrahydrofuran type-lignans from

Myristica fragrans

13C-NMR

Compound 7

Trang 16

O HO

MeO

OH OMe

O

O HO

MeO

OH OMe

O HO

MeO

OH OMe

O

O O

2'

4' 5' 6'

2'' 3'' 4'' 5'' 6''

Fig 3 Chemical structures of compounds 1–7 isolated from Myristica fragrans

Trang 17

Processing procedures for reducing myristicin contents from extracts

Mob Phase: EtOH:H2O

60% EtOH 80% EtOH 90% EtOH 100% EtOH Aceton

Trang 18

Processing procedures for reducing myristicin contents from

extracts of Myristica fragrans

Step 1

0 50 100

Minutes c:\gilson\test\test-1.009\test-1.gdt : uv1 : Step 1: Inj Number: 1

c:\gilson\test\test-1.009\test-1.gdt : uv2 : Step 1: Inj Number: 1 pump a

pump b

3

1

2 4

5

6

7

Fig 18 A representative HPLC profile of some major lignans (1–6) and myristicin from

the total MeOH extract of Myristica fragrans with detections at 205 and 280 nm Key to peak identity: (1) macelignan, (2) meso-dihydroguaiaretic acid, (3) (±)-trans-

dehydrodiisoeugenol, (4) nectandrin B, (5) licarin A, (6) otobaphenol, and (7) myristicin

Chromatographic method used: 0-40 min (50-70% MeOH), 40-52 min (70-100% MeOH), 52-60 min (100% MeOH)

Trang 19

Processing procedures for reducing myristicin contents from

extracts of Myristica fragrans

Step 3

0 50 100

Fig 19 A representative HPLC profile of isolated lignans 1−7 from the 80%

EtOH fraction of the 30% EtOH-soluble extract of Myristica fragrans with

detections at 205 and 280 nm Key to peak identity: (1) tetrahydrofuroguaiacin B, (2) saucernetindiol, (3) verrucosin, (4) nectandrin B, (5) nectandrin A, (6)

fragransin C1, and (7) galbacin (For chromatographic protocol see Experimental

and Methods)

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Table 4 Contents of nectandrin B and myristicin in each solvent

fraction from 30% EtOH-soluble extract of M fragrans

Table 3 Contents of nectandrin B and myristicin in each solvent

extract of M fragrans

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Effect of tetrahydrofuran type-lignans from Myristica fragrans

on AMPK activation

Fig 20 Stimulatory effects of isolated lignans 1−7 on AMP-activated protein

kinase (AMPK) activity (A) The stimulatory effects of isolated compounds 1−7

on AMPK activity at the concentration of 20 μg/mL (B) The stimulatory effects of g/mL (B) The stimulatory effects of

isolated compounds 1−7 on AMPK activity at the concentration of 5 μg/mL (B) The stimulatory effects of g/mL.

Trang 22

Animal experiment

Table 5 Characterization of ND mice as control with normal diet, and HFD

mice treated with or without THF for six weeks

Trang 23

Animal experiment

Trang 24

 AMPK - a therapeutic target for the treatment of metabolic syndrome

 seven 2,5-bis-aryl-3,4-dimethyltetrahydrofuran lignans were isolated

 Tetrahydrofuran mixture exert anti-obesity effect in C57BL/6 models

 Processing procedure to prepare a myristicin-free, lignan enriched fraction was established.

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