Χημεία Κρασιού.doc

  • Published on
    04-Jul-2015

  • View
    3.306

  • Download
    3

Embed Size (px)

Transcript

<ul><li> 1. : -Dicarbonyl (858) (861) 2010 </li></ul> <p> 2. . ...........2 ....................... 3 ... 4 .. 5 ........... 91. UV-VIS ...............9 ..........9 ......102. - (GC-MS) ... 11 .......... 113. (HPLC) .... 14 ...14 . 15 HPLC .... 15 .. 17 ....... 19 ... 22 ..... 23 ............................................................................................. 23 2 3. Tammy J. Dwyer Jeremiah D. Fillo San Diego, . . Assaying -Dicarbonyl Compounds in Wine: A Complementary GC-MS, HPLC, and Visible Spectrophotometric Analysis, Journal of Chemical Education (Vol. 83, No. 2, February 2006), , . - phenylenediamine (4) -dicarbonyl , :1) glyoxal (1)2) methylglyoxal (2)3) 2,3-butanedione (3) quinoxaline:1) quinoxaline (5)2) 2-methylquinoxaline (6)3) 2,3-dimethylquinoxaline (7) 1: -dicarbonyl -phenylenediamine quinoxaline .3 4. -phenylenediamine C6H4(NH2)2. . . 2,3-butanedione, diacetyl, C4H62 . , . 2,3-butanedione . glyoxal CHCH. . methylglyoxal (MG), pyruvaldehyde 2- oxopropanal, , , 1mM . , . MG . , MG glyceraldehyde-3- dihydroxyacetone MG . MG , . MG , MG , , MG ., MG . , MG :i) (GC-MS)ii) (HPLC) quinoxaline pyrazine . , .4 5. Tammy J. Dwyer Jeremiah D. Fillo : 500L 1,5mg -phenylenediamine Eppendorf , 30C, . , quinoxaline : 1) , 30, 5 . quinoxaline, 2-methylquinoxaline 2,3-dimethylquinoxaline . max , . Thermo-Spectronic UNICAM UV500. , quinoxaline max=315nm. ( 9), . 9 : -phenylenediamine. Sauvignon blanc (Amper Hill) Chardonnay (Sutter Home &amp; Charles Shaw).5 6. 2) (GC-MS), 3 5 30 . 1L GC-MS. 60C 2C/min 120C ( ). , 15C/min 230C, 5 . Single Ion Monitoring (SIM: ) . SIM, , 45. 2-methylquinoxaline methylglyoxal , 10 quinoxaline 1. 10 : ( ): , , methylglyoxal ( -phenylenediamine 2-methylquinoxaline). SIM. ( ): X 2-methylquinoxaline .6 7. 1 : quinoxaline GC-MS. 3) (HPLC), 2 5 10 . reverse-phase C18 (Waters 610E HPLC Higgins Analytical CLIPEUS 5-m). 50:50 : (0.040 , pH 4) 315nm. 5*10-7 2*10-5, quinoxaline ( 11). 11 : HPLC : quinoxaline, 2-methylquinoxaline 2,3-dimethylquinoxaline. 7 8. glyoxals quinoxalines , 12. 12 : HPLC - phenylenediamine: () Chardonnay, () Sauvignon Blanc, () Cabernet Sauvignon, () Merlot. ( ) 5.2 min (quinoxaline), 5.7 min (2-methylquinoxaline), 6.1 min (2,3-dimethylquinoxaline). , 5.210.01sec quinoxaline, 5.610.06min 2-methylquinoxaline 5.990.20min 2,3-dimethylquinoxaline. quinoxaline , 2. 2 : quinoxaline HPLC. 8 9. - I. UV-VIS, , UV-VIS, , , , , , .. : , , , . , , , , . , . , , . , UV-vis (UV : 190-400nm), (visual 400-800nm), , , , . : 2: UV-vis.9 10. Hg, H2, (D) (W) . (, ), , . , . , UV, VIS. 1 2 . , . , , . , ( ) , . :) , . . ) , (blank), , . . , . ) , (calibration curve), ( %), . . % 10% , ( = 1). 10 11. II. - (GC-MS) . , , .. - , (S) . ( ) , (m/z) . () . : 3: . (GC) ( 2, e, H2, Ar) , , . . T . .11 12. , , . , , . . , , . , . . . . , U, , , , , , 1-2 m , , mm , cm . , 1L , (septum). H . , . , . , . . (MS) : 1. , , , 2. , (m/z), 3.To . 12 13. 4: . . , . . , (3000-4000 gauss) . . . , ( 70eV), , . , m/z. 5: .13 14. : (CI), (FI), Xe Ar Cs (FIB). : , , , . III. (HPLC) HPLC , , . HPLC : I. , , , II. , . , . : :i. ii. , iii. iv. .v. . , () .14 15. Rs , k . k . , ( ), , : 1 &lt; k &lt; 20. : HPLC . , , . , , ppb. HPLC . . HPLC : HPLC , . i) . . , . :15 16. a. , ( SiO2 Al2O3) , , .b. , , , (, ), , , , .., ( ,, ..) .ii) , .iii) . , , p, . iv) , , . , .16 17. v) . , , , . : : 1. (pump).2. (injector valve).3. (column).4. (detector).5. .6. - . 6: HPLC. , . (isocratic), (gradient) . , . 17 18. , , , . , , . (, ), 6000 psi (~ 400 Atm) . . , . (isocratic elution) (gradient elution) , . . , , . . . , . . . (columns): HPLC , , . 10-50 cm 1-5mm. . 18 19. . 400 5-10m. "" , , . : ) , ) . ( ) : 1) 5-10m . 2) &gt;60m . 3) 35-45m, . HPLC : - -- - - - - - - - - :1) k :t R t0 k t0 tR ( 19 20. ) t0 ( ). 2) , . , .kB kA3) :2 t N 16 R W W .4) : LHN L . 7 : .5) RS . , . :tB t A RS 2 W A WB tA tB WA, WB . 20 21. , , : 1 a 1 RS 4 1 k N 1 k 8 : .21 22. quinoxalines -phenylenediamine glyoxal, methylglyoxal 2,3- butanedione , quinoxaline. , GC-MS quinoxalines o- phenylenediamine glyoxals. , quinoxalines , . HPLC . GC-MS HPLC glyoxals . , 2. , 2,3-butanedione ( ) . -dicarbonyl : glyoxal, methylglyoxal, 2,3-butanedione, . , ( Chardonnay) - dicarbonyl , Riesling. , -dicarbonyl. , glyoxal, methylglyoxal 2,3-butanedione . glyoxal2.7 10 5 3.8 10 5M 6.2 10 6 7.6 10 5 M 2-methylglyoxal9.0 10 6 4.0 10 5 M 1.5 10 6 4.0 10 5 M2,3-butanedione2.3 10 6 3.3 10 5 M 1.0 10 5 5.8 10 5 M 3 : -dicarbonyl . 22 23. 1. Assaying of -Dicarbonyl Compounds in Wine: A ComplementaryGC-MS, HPLC, and Visible Spectrophotometric Analysis, Tammy J.Dwyer and Jeremiah D. Fillo, Journal of Chemical Education, Vol.83, o 2, February 2006. 2. , , , 2006. 3. , , , 2003. 1. http://chimikoergastirio.blogspot.com/2009/12/hplc.html 2. http://chimikoergastirio.blogspot.com/2008/09/uv-vis.html 3. http://chimikoergastirio.blogspot.com/2009/11/s.html 4. http://www.chem.uoa.gr/courses/organiki_1/fasm_org/Chapter_11.pdf 5. http://www.chem.uoa.gr/courses/analtechn/SAT_02_Mass_Spectrometry_pt1.pdf 6. http://www.chem.uoa.gr/courses/analtechn/SAT_03_Mass_Spectrometry_pt2.pdf 23 </p>

Recommended

View more >