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applications ?
Advantages of Purospher® STAR and Chromolith® HPLC columns in
quality control
Page 2
Silica Gel Production Plant - Gernsheim
Page 4
LiChrosorb, LiChrospher, Superspher
Reversed phase modified silica gels for RP-Chromatography
Specifications
Sorbents Particle Pore Pore Spec. % C Surface Efficiency (N/m)
size size volume surface coverage
(µm) (Å) (ml/g) area (µmol/m2)
(m2/g)
LiChrosorb® RP-8 5, 10 100 1,0 300 9,5 3,4 55.000, 20.000
LiChrosorb® RP-select B 5, 10 60 0,75 300 11,4 4,21 55.000, 20.000
LiChrosorb® RP-18 5, 10 100 1,0 300 16,2 3,0 55.000, 20.000
LiChrospher® RP-8 5, 10 100 1,25 350 12,5 4,04 55.000, 25.000
LiChrospher® RP-8e 5, 10 100 1,25 350 13,0 4,44 55.000, 25.000
LiChrospher® RP-select B 5, 10 60 0,9 360 11,5 3,55 55.000, 25.000
LiChrospher® RP-18 5, 10 100 1,25 350 21,0 3,61 55.000, 20.000
LiChrospher® RP-18e 5, 10 100 1,25 350 21,6 4,09 55.000, 20.000
Superspher® RP-8 4 60 1,25 350 12,5 4,04 100.000
Superspher® RP-8e 4 60 1,25 350 13,0 4,44 100.000
Superspher® RP-select B 4 60 0,9 360 11,5 3,55 100.000
Superspher® RP-18 4 100 1,25 350 21,0 3,61 100.000
Superspher® RP-18e 4 100 1,25 350 21,6 4,09 100.000
Page 5
LiChrospher® 60 RP-select B (5 µm)
2 2
2 3
1 4
5
6 4
1
Batch 1
Batch 2
Batch 3
Batch 4
Batch 1
Batch 2 L551205
Batch 3 Batch 5
Batch 4 Batch 6
Batch 5
Batch 6 Batch 7
Batch 7
Batch 8 Batch 8
Batch 9
Batch 10 Batch 9
Batch 10
Page 7
LiChrospher® RP-select B
Reproducibility
Tanaka 1 - Test:
L56049418Nr.
601919
L56038218 Nr.
601914
L55120518 Nr.
601895
Page 8
LiChrospher® RP-select B
Reproducibility
Eluent: Methanol/Wasser 30/70
Tanaka 2 - Test: Fluß: 1mL/min
Inj.v.: 5L
Det.: UV254nm
Temp.: 22°C
Probe: 0,01mg/mL Uracil
0,022mg/mL Coffein
0,09mg/mL Phenol gelöst in MeOH/W
30/70
B4186/04 No.601926
L56014218
No.601906
L55057818 No.601874
L55057718
No.601868
No.601857
L55057418 No.601849
L55057318 No.601813
L55057218
No.601804
Page 9
Column hardware
Hibar RT LiChroCART
Ready-to-use Cartridge column
column
Complete column with Cartridge with no
endfittings endfittings (special
cartridge holder - manu-
CART - is necessary)
Cost savings
Page 10
Purospher®® RPRP--18 18 endcappedendcap
Chelating Agents
O OH O OH
OH
2.
O OH O OH
Purpurin Quinizarin
0 5 10
Chromatographic conditions:
Page 11
Purospher ®
Purospher® 1 1 1 3 1
Purospher® STAR
Page 12
Metal impurities of silica gel manufactured
by conventional process
Na + - O OH free
Si Si
OH
- Si
O Si geminal
Fe2+ OH
-
O Si Si O H
OH
OH OH
atrix Si O H vicinal
OH Me OH
M
O
Si O Si Si
O O O O
O O
Si O Si O Si O Si
Page 13
Purospher ®
Type A Type B
Si (OC2H5)4
M2O - nSiO2 M=
Na, K, Fe
[-Si (OH)2 - O - [-Si (OC2H5)2 - O -
Si (OH)2- O -]n Si (OC2H5)2 - O
-]n
- Si - O - Si - O - - Si - O - Si - O -
O O O O
- Si - O - Si - O - - Si - O - Si - O -
n n
Page 14
Purospher ® RP-18 endcapped
Application Procainamides
3
0 7,5 15
Page 15
LiChrospher® RP-18 endcapped uses
conventional surface modification
OH
OH monofunctional
Si
O modification
Si OH CH3 CH2
CH2 CH2 CH2 CH2 CH2
O
Si
X Si CH2 CH2 CH2 CH2 CH2 CH2 C6H13
OH CH3
O
O Si
OH
Free silanol-groups are still
OH CH3 accessible after
CH3 OH
O Si O Si endcapping. Polar
Si
O
CH3 Si
O
CH3
CH3 interactions are still
Endcapping Si CH3
Si OH Si O possible.
OOH O OHCH3
Si O CH3 Si CH3
O
O Si O OH Si
O Si CH3 O Si CH3 CH3
OH O
Si CH3
CH3
Page 16
Purospher® STAR RP-18 endcapped
OH O
O
polymeric
Page 17
Purospher® STAR RP-8 endcapped
Separation of caffein & derivatives
Page 18
Purospher® STAR RP-18 endcapped
Separation of Cefazolin
Cefazolin
Chromatographische Bedingungen
Page 19
Purospher® STAR RP-18 endcapped
Highest pH Stability from 1.5 to 10.5
Purospher® STAR RP-18 endcapped, 5 µm, 150-4.6 mm with acetonitrile / water (0,1 % NH3 [25%]; 60:40), 1.0 ml / min at UV
254 nm
Sample: 1. Thiourea, 2. Benzene, 3. Toluene, 4. Propylbenzene, 5. Butylbenzene
Page 20
Merck Chromatography
- Development of Silica Gels
LiChrosorb® irregular
LiChrospher®
Superspher®
Purospher® spherical
Purospher® STAR
Chromolith® monolithic
Page 21
Chromolith® HPLC Columns
Page 22
Preparation
Si(OAlk)4
Polymer
H+
HPLC
Cladding
Page 23
The Bimodal Pore Structure
SEM of a cross
section of a
silica monolith
Mesopores: 130 Å
Macropores: 2m
Page 25
Page 26
Chromolith® HPLC columns are robust
Page 27
Chromolith® Specification
Page 29
Column back-pressure
3µm and 5µm columns
250
3.5 m
200
5 m
150
100
50 Chromolith® Performance
0
0 2 4 6 8 10
1
4 Chromolith® Performance RP-18e
3 5 100 mm x 4.6 mm
5 ß-Blocker
1 mL/min - 17 bar
Mobile Acetonitrile/
0.1% TFA in
3 mL/min - 51 bar water
Phase (20(80; v/v)
Flow rate 1-9 ml/min
Detection 222 nm
Sample 1. Atenolol
2. Pindolol
9 mL/min - 153 bar 3. Metoprolol
4. Celiprolol
5. Bisoprolol
Page 32
Speed and Quality in Practice
2
2
1
4 1
3 4
5 3 5
0.0 1.5
1 mL/min - 17 bar
12
9 mL/min - 153 bar
Page 33
Chromolith® HPLC Columns
- unique properties and benefits (1)
Page 34
Chromolith® HPLC
Page 35
High throughput analysis with monolithic
silica columns
Chromatographic conditions:
Page 36
Chromolith® HPLC Columns
- unique properties and benefits (2)
Page 37
Chromolith® HPLC Columns
- Higher Separation Efficiency
6
6
Page 38
Chromolith® HPLC Columns
- unique properties and benefits (2)
Page 39
Chromolith® HPLC Products
1.51467.0001
Chromolith Column Coupler
Page 40
Chromolith® HPLC Columns
- unique properties and benefits (3)
Page 41