Академический Документы
Профессиональный Документы
Культура Документы
1
3/6/2018
http://mrswolfgang.wikispaces.com/file/view/photoggggg.jpg/65003922/512x384/photoggggg.jpg
http://www.labsource.com/ProdImg/14/14320.jpg
2
3/6/2018
3
3/6/2018
Watson, 1999
Pharmaceutical Analysis,
Churcill Livingstone,
Page 77
4
3/6/2018
5
3/6/2018
Luminescence Phenomena
Organic fluorescence indicators for aluminium oxide, silica gel and cellulose layers
(code F366, UV366) include:
• the sodium salt of 3-hydroxypyrene-5,8,10-trisulfonic acid
• the sodium salt of 3,5-dihydroxypyrene-8,10-disulfonic acid
• sodium fluorescein and fluorescein or 2',7'-dichlorofluorescein
• rhodamine B and rhodamine 6G
• Morin
• cyanine dyestuffs
• stilbene derivatives (e.g. diaminostilbenetriazine) and
• optical brighteners (Ultraphor WT BASF, Calcofluor R-white, Leukophor).
6
3/6/2018
7
3/6/2018
Normal phase :
Polarity of stationary phase > mobile phase
Stationary phase : silica
Mobile phase : non polar organic solvents
Reversed phase :
Polarity of mobile phase > stationary phase
Stationary phase : RP-18
Mobile phase : water-based mobile phase
Adsorption chromatography:
Adsorption in TLC occurs at the surface of the particles of
the stationary phase, which are in contact with the mobile
phase
Partition chromatography :
In partition chromatography, separation depends on the
relative solubility of the sample components in two immiscible
solvents brought into contact with each other
8
3/6/2018
(Komsta, 2007)
9
3/6/2018
Sampel Sampel
preparation application
Prechromatographic
Derivatization steps
Postchromatographic
Visual and
photometric
examination
Chromatogram
–detection-
Chromatographic
development
10
3/6/2018
Sampel Sampel
preparation application
Prechromatographic
Derivatization steps
Postchromatographic
Visual and
photometric
examination
Chromatogram
–detection-
Chromatographic
development
11
3/6/2018
O
H2N
OH
GABA
O H2C
O H2N
H2N O
H3C OH
H2N
OH
CH3 OH
Gabapentin Vigabatrin
Pregabalin
HO
O
H2N O O
OH
H
S
Gabapentin H
O
N HO
O
O OH O
H2N o-phthalaldehyde
H3C OH
S
CH3 O
O HO N
Pregabalin
O OH
H3C
HS OH
H2 C CH3
3-mercaptopropionic acid CH2
S
O
H2N O
N
OH
OH
Vigabatrin
12
3/6/2018
ABSORBANCE VS REFLECTANCE
Calculation of Rf-value.
• Spot 2 has an identical Rf and
color with standard 1 (St 1), but
it does not mean that spot 1 was
always identical with St 1.
13
3/6/2018
Z6 – Z0
Rf Z6 =
Zf – Z0
14
3/6/2018
(Spangenberg, 2011)
15
3/6/2018
(Dünnschichtchromatographie) = TLC
OH
OH
HO O
OH
OH O
Rutin
(major active components in Ginkgo biloba)
Mobile phase:
Ethyl acetate : acetic acid : formic acid :
water (100:11:11:26)
Stationary phase:
HPTLC plates silica 60 F254
16
3/6/2018
TERIMA
KASIH
octadika@yahoo.com dika_octa
17