Post on 11-Jan-2016
description
Chiral Technologies Development Ltd.Rumbach S. 7., Budapest, H-1075, Hungary
Phone: 36-1-352-2405 Fax: 36-1-413-6944
E-mail: chiroquest@chello.hu web: www.chiroquest.org
Chemically bonded 4-nitrophenyl-urea stationary phases
π-Select•high surface coverage
•fully endcapped
CD-Screen•optimized coverage, according to the size of cyclodextrin molecule
•free silanols
N+
O-
O
NH
OO
NHCH2CH2CH2
O
O Si
H-acceptor
H-donors
δ+
hydrophylic hydrophobic
DIMETHYL-PHTALATE
click on image for animation
CAFFEINE
click on image for animation
PHENOL
click on image for animation
min0 2 4 6 8 10 12 14 16 18
mAU
0
5
10
15
20 1
2
min0 2 4 6 8 10 12 14 16 18
mAU
0
5
10
15
20
25
12
π-Select
Conventional phenyl-column
Eluent: MeOH-water 30:701.: Phenol2.: Caffeine
k’=0.54
k’=0.25
Polar analytes
min0 2 4 6 8
mAU
0
2.5
5
7.5
10
12.5
15
17.5
20
2
3 4
1
min0 2 4 6 8
mAU
0
100
200
300
400
500
600
700
800
1
2+3
4
π-Select
Conventional phenyl-column
Eluent: MeOH-water 60:401.: Dimethyl-phtalate; 2.: Diethyl-phtalate3.: Biphenyl 4.: o-Terphenyl
C: 4.7%
C: 7.0%
Apolar, aromatic analytes
*
Tyr-Pro-Phe-Atc-NH2
Eluent: 0.1% TFA in water-0.1% TFA in MeOH 75:25Atc-NH2: 2-amino-decaline-2-carboxylicacid
* : racemic amino acid
min0 2 4 6 8 10
mAU
0
20
40
60
80
100
1
2
3
4
Eluent: MeOH-0.1% H3PO4 60:40 0.8 ml/min pH: 2.61.: N-methyl-ephedrine; 2.: Athenolol3.: Pindolol; 4.: Sertraline
Diastereomer peptides
Basic drugs
Separation of Polinuclear Aromatic Hydrocarbons on Pi-Select column
S
S
1. Benzothiophene
4. Dibenzothiophene
7. Benzo[g,h,i]perylene
6. Benzo[a]pyrene
3. Fluoranthene
2. Fluorene 5. Pyrene
[min.]Time
0 1 2 3 4 5 6 7
[mV]
Vol
tage
0
200
400
600
800
TOH_MeOH_85_ism
1
2 3
6 7
[min.]Time
0 2 4 6 8
[mV]
Vol
tage
0
100
200
300
400
500
600
ToL_MeOH_70
12
4
35
methanol-water 85:15 methanol-water 75:25
Prostaglandine intermediate
min0 2.5 5 7.5 10 12.5 15 17.5 20
mAU
0
50
100
150
200
min0 2.5 5 7.5 10 12.5 15 17.5 20
mAU
-10
0
10
20
30
40
Plates: 16685
Asymmetry: 1,189
Plates : 5649
Asymmetry : 1,261
π-Select
LiChrosphere Si 60
Eluent: n-hexane - TBME 97:3
*
R
O
O O Si
COOCH3
cis and trans
R and S
1.: dehydroepiandrosterone2.: testosterone3.: androstenedione4.: pregnenolone5.: dehydroepiandrosterone-sulfate
O
CH3
CH3
O
H HH
H
Steroids in blood
Juvenile hormone (insecticide) geometrical isomers
CD-SCREEN
Inclusion complex with beta-cyclodextrin
click on image for animation
min2 4 6 8 10 12 14 16 18
V
30
35
40
45
50
55
60
65
70
ADC1 A, ADC1 (D:\TESZTEK\REPROD\CDT0218B\HPBCD351.D)
Hydroxypropyl-β-CDthe most likely candidate for incorporation into various drug formulations
2 4 6 8 10
50
100
150
200
250
300
350
β-CD
.
Nucleosil 120-7 NH2 column, normal phase
•solubility problems
•β-CD contamination is the last peak, the integration is difficult
•poor resolution of isomeric groups
CD-Screen column, reversed phase
•good solubility in the eluent
•β-CD contamination is the first peak, high accuracy analysis is possible
•detailed „fingerprint” chromatogram
β-CD
min10 20 30 40 50
Norm.
90
100
110
120
130
BC
D
Sto
p t
ime 1
2 m
in.
min5 10 15 20 25
mV
0
20
40
60
80
100
BC
D
Sto
p t
ime
, is
oc
rati
c
min2 4 6 8 10 12 14 16 18
V
20
30
40
50
60
BC
D
60 min.
20 min.
TNP: 1800/m
TNP: 32000/m
USP method for analysis of Hydroxypropylbetadex
Alternative method on CD-Screen column
min5 10 15
mV
150
200
250
300
350
400
Bomlástermékek
RAMEB
Randomly methylated β-CD
Degradation products
min2 4 6 8 10 12 14 16
mV
50
100
150
200
250
300
350
400
Randomly methylated α-CD
α-CD
-SelectDiametrically Different Retention Mechanism
Unique Selectivity
•Good alternative when current C18 fails to deliver•Diametrically different selectivity to other reversed phase columns•Embedded H-donor and H-acceptor groups•High retention of aromatics due to - interactions•Excellent shape-selectivity•100% water can be used as eluent, no collapse•High polarity reversed phase•A single column can be used in reversed and normal phase separations •Based on “B”-type, High Purity Silica, fully endcapped•Available with 3m and 5m particle size for analytical purpose, and 10m particle size for preparative applications.
For more information please visit our web pages: www.chiroquest.org