반응 #2460280

ord-bdb00d7604734fb8a5cf21e566112010

반응 방정식

CCCCCCCCCCCCCCCC(=O)OC/C=C(C)/C=C/C=C(C)/C=C/C1=C(C)CCCC1(C)C
retinyl palmitate
C[O-].[Na+]
sodium methoxide
FB(F)F
boron trifluoride
O
water
CC(C[*:1])[*:2]
polypropylene
CC(C=CC1=C(C)CCCC1(C)C)=CC=CC(C)=CCOC=O
Retinyl Esters

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The mixtures were placed in a shaking water bath at 55° C. for 20 or 23 hours
  2. 2
    기타The immobilised lipase was then removed by simple filtration
  3. 3
    기타to directly yield the product
  4. 4
    기타The composition of the retinyl esters was separated from the triglycerides by thin layer chromatography (0.5 mm silica G plates, Analtech Ltd.)
  5. 5
    세척as eluting solvent
  6. 6
    기타FAMEs were produced
  7. 7
    기타at 80° C.
  8. 8
    기타for 20 minutes
  9. 9
    기타PTV injection (Run: 3 min @ 260° C., 80° C. hold 1 min, +20/min to 180° C., +2/min to 220° C., +1/min to 230° C., +4 min hold at 230° C.)

실험 절차

Sunflower oil (7.5 g) and retinyl palmitate (2.5 g) were mixed and water (0.03 g) and immobilised Lipase D (Rhizopus oryzae (Amano) immobilised on Accurel® EP100 macroporous polypropylene (Acordis) 0.1 g) or Candida rugosa AY (Amano) on Accurel® EP100 (Acordis) (CR; 0.1 g) added. The mixtures were placed in a shaking water bath at 55° C. for 20 or 23 hours. The immobilised lipase was then removed by simple filtration to directly yield the product, a solution of retinol esters in triglyceride oil. The composition of the retinyl esters was separated from the triglycerides by thin layer chromatography (0.5 mm silica G plates, Analtech Ltd.) using toluene as eluting solvent and visualised by spraying with 1% 2,7-dichlorofluorescein in ethanol. The ester band was scraped off and FAMEs were produced using 3 ML sodium methoxide and 1 mL toluene at 80° C. for 20 minutes followed by 5 minutes at 80° C. with boron trifluoride (2 mL volumes of reagent). The fatty acid content was then analysed by Fatty acid methyl ester Gas Chromatography (FAME-GC). GC conditions: Column—30 m/0.53 mm/0.5 um restek famewax, Helium carrier gas 15 kpa, flame ionisation detection, 260° C. PTV injection (Run: 3 min @ 260° C., 80° C. hold 1 min, +20/min to 180° C., +2/min to 220° C., +1/min to 230° C., +4 min hold at 230° C.).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07459288B2uspto-grants-2008_12