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1. Introduction(abstract)
- page 1
2. LC-MS
- page 1
3. NMR
- page 3
4. NMR°ú LC-MS¸¦ ÅëÇÑ ÈÇнÄÀÇ ÃßÃø
- page 6
5. NMRÀ» ÅëÇÑ ºÐÀÚ±¸Á¶ÀÇ ÃßÃø
- page 10
6. GC-MS
- page 15
7. HPLC
- page 19
8. Summary& Discussion
- page 23
9. Reference
- page 25
1. Introduction(abstract)
±â±âºÐ¼® ¼ö¾÷À» ÅëÇÏ¿© ¿©·¯ °¡Áö ºÐ¼®¹ýÀÇ ¿ø¸®¿Í ±× ÀڷḦ Çؼ®ÇÏ´Â ¹æ¹ýÀ» ¹è¿ì°Ô µÇ¾ú´Ù. ±× ¼ö¾÷ ³»¿ëÀ» ¹ÙÅÁÀ¸·Î ÇÏ¿© ½ÇÁ¦ NMR HPLC LC-MS GC-MS Àåºñ¸¦ ÀÌ¿ëÇÏ¿© ÁÖ¾îÁø ¹ÌÁöÀÇ ¹°ÁúÀ» Á¤·®, Á¤¼º ºÐ¼®ÇÏ¿© ¹°ÁúÀÇ ±¸Á¶¿Í ¼ºÁúÀ» ¹àÇô³»°í ÀÌ ¹°ÁúÀÌ ¹«¾ùÀÎÁö¿¡ ´ëÇؼ ¾Ë¾Æº»´Ù. ¶ÇÇÑ ÀÌ·¯ÇÑ °úÁ¤¿¡¼ ±â±âºÐ¼®À» ÅëÇØ ¾òÀ» ¼ö ÀÖ´Â Á¤º¸µéÀÌ ¹«¾ùÀÎÁö ¾Ë¾Æº»´Ù.
2. LC-MS
1) METHOD
¡Ú Sample preparation
1. Dissolve 1mg of sample in 1ml of DMSO in eppendorf tube
2. Filtration with 0.2 ¥ìm GHP membrane filter
3. Dilution w¡¦(»ý·«)
2) RESULT ANALYSIS
¨ç ES- 227/ES+ 229
¨è ES- 456/ES+ 455
|
455
ES- : 456 -H= 455
ES+: 454 +H= 455
°°Àº ¹æ½ÄÀ¸·Î °è»êÇغ¸¸é ES-ÀÏ ¶§ÀÇ ¹°ÁúÀÇ MW´Â 454, ES+ÀÏ ¶§ÀÇ MW´Â 456À¸·Î ¼·Î ºÒÀÏÄ¡ÇÏ¿© ÀÌ ÇÇÅ©´Â ¿ì¸®°¡ ¿øÇÏ´Â ¹°ÁúÀÇ MW°¡ ¾Æ´Ï¶ó°í ÃßÃøÇÒ ¼ö ÀÖ´Ù.
3. NMR
1) METHOD
¡Ú Sample preparation
1. sample(about 10mg) dissolve in NMR solvent(Deuterated solvent) - minimum 600ul : NMR solvent ´Â metanol peak ¸¸ ¶ß´Â ¹®Á¦°¡ ÀÖÀ¸¹Ç·Î Áß¼ö¼ÒÈ ÇÏ¿© NMR¿¡ ÃøÁ¤ ¾È µÇ´Â ¿ë¸Å¸¦ »ç¿ë.(99.95% Áß¼ö¼ÒÈ)
2. sample put in NMR tube
3. NMR analysis
- Locking (ÀÚÀåÀÇ ¾ÈÀü¼ºÀ» È®º¸Çϱâ À§ÇØ - To find z0)
- Shiming (ÀÚÀåÀÇ ±ÕÇü¼ºÀ» È®º¸Çϱâ À§ÇØ)
- Tunning (ÁÖÆļö¸¦ Àß Àâ±â À§Çؼ)
- Running
- Data processing
4. Get 1D and 2D NMR spectrum & HPLC, LC/MS, GC/MC data
5. Determination of compound structure.
2) H-NMR RESULT ANALYSIS
¸ÕÀú H-NMRÀÇ chemical shift¿Í ÇÇÅ©ÀÇ ÀûºÐ °ªÀ» ÅëÇÏ¿© ¹°ÁúÀÇ ´ë·«ÀÇ ±¸Á¶¿Í HÀÇ °³¼ö¸¦ ã¾Æº»´Ù. sampleÀÇ chemical shift °ªÀº 6.16ºÎÅÍ 7.36 Á¤µµ¿¡ ¸ô·Á ÀÖÀ½À» º¼ ¼ö ÀÖ´Ù. ¸¦ ÂüÁ¶Çϸé ÀÌ °ªµéÀº ¸ðµÎ c=c-H ȤÀº Aromatic Ring ÀÇ chemical shift¹üÀ§¿¡ Æ÷ÇԵȴÙ. µû¶ó¼ ÀÌ ¹°ÁúÀÇ ±¸Á¶°¡ ÀÌÁß°áÇÕ°ú Aromatic RingÀ» °®´Â´Ù°í »ý°¢µÈ´Ù.
´ÙÀ½À¸·Î ÀûºÐ °ªÀ» ÅëÇÏ¿© HÀÇ °³¼ö¸¦ ã¾ÆÁØ´Ù. ÀÓÀÇÀÇ ±âÁØ ÇÇÅ©ÀÇ Area °ªÀ» 1·Î Àâ°í