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The moment you adopt our Kromasil High Performance Concept, you join thousands
phases for better performance
PUBBankv_1105
of chromatographers who share a common goal: to achieve better separations when
analyzing or isolating pharmaceuticals or other substances.
Not only will you benefit from our patented silica technology, but you gain a
strong partner with a reliable track record in the field of silica products. For the past
60 years, Eka Chemicals has pioneered new types of silica. Our long experience in
This publication may not be reproduced in any way without the consent of Eka Chemicals AB.
the field of silica chemistry is the secret behind the development of Kromasil, and
the success of our Separation Products Group.
Kromasil is available in bulk, or in high-pressure slurry-packed columns.
The development, production and marketing of Kromasil are ISO 9001 certified.
Eka Chemicals is a global company with 3,000 people in 30 countries. It is a business
unit within AkzoNobel, one of the worlds largest chemical groups, with more than
67,000 employees in 80 countries.
Kromasil AmyCoat
Kromasil CelluCoat
www.kromasil.com Kromasil
Designed to stretch the limits.
Kromasil AmyCoat and Kromasil CelluCoat stretch the limits for analytical
and industrial chiral chromatography. The silica is based on an in-house developed
matrix and coated with a functionalized amylose or cellulose selector. High resolution,
excellent selectivity, no pressure limits* and stable performance when switching
between compatible mobile phases are some important benefits.
Analytical chromatography
Preparative chromatography
* Kromasil AmyCoat and Kromasil CelluCoat can withstand flow rates equivalent to
pressures of up to 400 bari.e. the approximate limit for most HPLC systems.
Peak performance. Expect nothing less. Kromasil AmyCoat Kromasil CelluCoat
Selectivity and resolution comparisonKromasil AmyCoat 3 m and Chiralpak AD-H (5 m). Selectivity and resolution comparisonKromasil CelluCoat 3 m and Chiralcel OD-H (5 m).
Kromasil AmyCoat, 3 m Chiralpak AD-H
Rs Kromasil CelluCoat, 3 m Chiralcel OD-H
Rs
To speed up and simplify method development, we have removed some of the 500
= 1.5
800 0
= 1.5
AmyCoat 3 m Chiralpak AD-H* AmyCoat 3 m Chiralpak AD-H* 500
= 2.3
400 0
= 2.0
CelluCoat 3 m Chiralcel OD-H* CelluCoat 3 m Chiralcel OD-H*
00
Rs= 7.3 605 0 Rs= 5.8 Ambucetamide 1.4 1.4 4.8 4.2 Rs= 13.2 305 0 Rs= 8.3 Trans-Stilbene oxide 2.3 2.0 13.2 8.3
restrictions for coated polysaccharide phases. In analytical scale chromatography, 000 Carbinoxamine 1.5 1.5 7.3 5.8
50
0 Benzoin 1.5 1.5 8.6 5.7
400 0 Ketoprofen 1.4 1.3 4.6 4.3 200 0 TFAE 2.9 2.9 14.7 11
3 m particles and the absence of pressure limits allow faster chromatography with 0
50
Naproxen 1.2 1.2 3.4 3.1 00
0
Trgers base 1.4 1.4 3.7 2.7
205 Oxamniquine 1.2 1.2 3.3 3.1 105 Oxprenolol 5.6 5.5 18.1 15.1
50
better results than ever before. 0 0
Proglumide
Sulindac
2.7
1.3
2.8
1.3
11.8
4.8
9.0
3.9 0 0
Naproxen
Proglumide
1.2
2.0
1.2
2.0
2.9
7.6
2.2
3.2
0 5 10 15 0 5 10 15 (* 5 m) 0 2 4 6 8 0 2 4 6 8 * (5 m)
[min.] [min.] [min.] [min.]
Both Kromasil AmyCoat and Kromasil CelluCoat Not only can you get better results with Kromasil
show great enantioselectivity for many different AmyCoat and Kromasil CelluCoat you also get
racemates. In a separate section of the brochure, them faster. Thanks to a product characteristic
you will find an application guide showing exactly like the absence of pressure limits, you can run
the performance levels you can expect. analytical chromatography at very high flow
By having access to 3 m particles, it enables rates and save time. Difference in resolutionKromasil AmyCoat Fast analytical chromatography Fast analytical chromatography
a higher plate count and resolution for analytical The high selectivity and 3 m particles are also 3 m vs. 5 m.
chromatography. Combined with great selectivity, important factors in speeding up the method. You Particle size: 5 m Particle size: 3 m Particle size: 3 m Particle size: 3 m Particle size: 3 m Particle size: 5 m Particle size: 3 m Particle size: 3 m Particle size: 3 m Particle size: 3 m
Column length: 150 mm Column length: 150 mm Column length: 150 mm Column length: 150 mm Column length: 150 mm Column length: 250 mm Column length: 150 mm Column length: 50 mm Column length: 50 mm Column length: 50 mm
this facilitates the separation of the enantiomers. achieve an improved resolution, which, in turn, .4
4
Flow rate: 1 ml/min
.5
Flow rate: 1 ml/min Flow rate: 1 ml/min Flow rate: 2 ml/min Flow rate: 4.5 ml/min Flow rate: 1 ml/min Flow rate: 1 ml/min Flow rate: 1 ml/min Flow rate: 3 ml/min Flow rate: 7 ml/min
0
allows a higher flow rate. 0 = 1.1 = 1.1 00 00 00 50 00 00 00 5
.3
.4 =2.3
= 1.8
= =2.21.8 = 1.7 = 2.2 = 2.3 = 2.3 = 2.2 = 2.2
Rs= 1.3 Rs= 2.1 Rs=R4.7
= 6.9 R = 5.6 Rs= 3.5
00 s 00 Rs=s 3.8 Rs= 9.0 Rs= 10.8 Rs= 4.7 Rs= 3.8 Rs= 3.0
00 50 50
0 .3 00 00 0 0
.2 00 00
.2 00 00 00
00 00
0
.1 50 00 5 0
.1 00 50 50
00 00
0 0 0 0 0 0 0 0 0 0
0 2 4 6 0 1 2 3 0 0.75 1.5 0 5 10 0 5 10 0 1 2 3 0 1 0 1
[min.] [min.] [min.] [min.] [min.] [min.] [min.] [min.]
Kromasil AmyCoat and Kromasil CelluCoat are Kromasil AmyCoat and Kromasil CelluCoat
available in particle sizes down to 3 m. faster results, better results.
CelluCoat high flow rate
selectivity
Kromasil AmyCoat and Kromasil CelluCoat let you perform method development with-
times and degradation in performance when switching from one compatible mobile 00
Rs= 15.5
1. Heptane/2-Propanol (90/10) 4.3 2 345 00
Rs= 15.6
90 2
After 100% 2-propanol (3h) = 2.1
0
1
2. 2-Propanol 0.7 2 260
phase to anotherthey simply do not exist anymore. 00 3. Acetonitrile 1 2 58 00
80
0 10 20 30 40 50
0
0
0 time [h]
1 0.1 0.2 0.3 0.4 0.5 0.6
4. Ethanol 1 2 188 Reduced velocity
0 5. Heptane/2-Propanol (90/10) 1 2 72 0 Conditions Common conditions
Solute: trans-Stilbene oxide Mobile phase: Heptane/2-Propanol (90/10) Solute: trans-Stilbene oxide Mobile phase: Heptane/2-Propanol (90/10)
0 5 10 0 5 10 Stationary phase: Kromasil CelluCoat, 3 m Flow rate: 7 ml/min Stationary phase: Kromasil CelluCoat, 5 m Flow rates: 0.1-1.2 ml/min
[min.] [min.] Column size: 4.6 x 50 mm Temperature: 25 C Column size: 4.6 x 250 mm Temperature: 25 C
No pressure limits Short equilibration times
Common conditions
User-friendliness, as we see it, is the ability to Column equilibration is a time-consuming activity Stationary phase: Kromasil AmyCoat, 3 m
Column size: 4.6 150 mm
Mobile phase: Heptane/2-Propanol (90/10)
Flow rate: 1 ml/min
Temperature: 25 C Detection: UV 229 nm
perform method development without being when running chiral chromatography. Higher flow
restricted by various parameters. One well-known rates allow Kromasil AmyCoat and Kromasil
restriction for coated polysaccharide phases is the CelluCoat to show substantially shorter equilibra-
general pressure limit over the bed. Kromasil tion times than other coated phases on the mar-
AmyCoat and Kromasil CelluCoat withstand flow ket. Short equilibration timesFreedom to switch solvents
Identical result Identical result
rates equivalent to pressures up to 400 bar In general, long equilibration times are most
which is about the limit for the HPLC system itself. pronounced when switching mobile phases Short equilibration timesFreedom to switch additives Mobile phase 1 Mobile phase 2 Mobile phase 1
50 50
50
This makes it possible to run analytical chromatog- containing basic additives to acidic additives or Identical result Identical result
00
= 2.3 00 = 1.4 00 = 2.2
Rs= 10.0 Rs= 2.6 Rs= 9.9
50 50
raphy a lot faster. the other way around. The test with a Kromasil Mobile phase 1
Solute: Carbinoxamine
Mobile phase 2
Solute: Ketoprofen
Mobile phase 1
Solute: Carbinoxamine
50
00 00
Detection: UV 228 nm Detection: UV 250 nm Detection: UV 228 nm 00 Equilibration Equilibration
CelluCoat 3 m column switching between two 00 00 00 50
Mobile phase 2 50
Duration: 10 min
Mobile phase 1 50
Duration: 15 min
= 1.5 = 1.2 = 1.5 0 0
Stable performance compatible mobile phases shows how short 00 Rs= 5.0
50
Rs= 3.4 00 Rs= 5.0
0
0 1 2 3 0 2 4
0 2 4 [min.] [min.]
[min.]
00
From a stability perspective, you can run Kromasil equilibration times you can get. 00 Equilibration Equilibration 00
Mobile phase 2 50 Mobile phase 1 Common conditions
AmyCoat and Kromasil CelluCoat using compatible There are also two tests illustrating short Duration: 18 min Duration: 12 min Solute: trans-Stilbene oxide
Detection: UV 229 nm
Column size: 4.6 x 150 mm
Mobile phase 1: Heptane/2-Propanol (90/10)
Flow rate: 2 ml/min
Temperature: 25 C
0 0 0
Stationary phase: Kromasil CelluCoat, 3 m Mobile phase 2: Ethanol
normal, polar organic and reversed mobile phases. equilibration times and additive switch for both 0 2 4
[min.]
0 2 4 6 8
[min.]
0 2 4
[min.]
Switching between compatible normal to polar Kromasil AmyCoat and Kromasil CelluCoat with
Common conditions
Stationary phase: Kromasil AmyCoat, 3 m Mobile phase 1: Heptane/2-Propanol/DEA (90/10/0.1) Flow rate: 2 ml/min
organic mobile phases will not lead to any deg- absolutely no sign of memory effects. Column size: 4.6 x 150 mm Mobile phase 2: Heptane/2-Propanol/TFA (90/10/0.1) Temperature: 25 C
0 0 0
0 2 4 6 8 10 0 2 4 6 8 0 2 4 6 8 10
[min.] [min.] [min.]
Common conditions
Stationary phase: Kromasil CelluCoat, 3 m Mobile phase 1: Heptane/2-Propanol/TFA (90/10/0.1) Flow rate: 1 ml/min
Column size: 4.6 x 150 mm Mobile phase 2: Heptane/2-Propanol/DEA (90/10/0.1) Temperature: 25 C
Works all the way. Kromasil AmyCoat Kromasil CelluCoat
Preparative applications Loadability comparison
Kromasil CelluCoat, 10 m Chiralcel OD, 10 m Kromasil CelluCoat, 10 m Chiralcel OD, 10 m
00 00
00 20
Carbinoxamine
10 00
0 0
0 5 10 15 0 5 10 15
0.9 g 0 0 0 0
Simplifies method development 4000 [min.] [min.] 0 5 10 15 20 25
[min.]
0 5 10 15 20 25
[min.]
0 5 10 15 20 25
[min.]
0 5 10 15 20 25
[min.]
Enantiomer 1 Enantiomer 2
With particle sizes from 3 m to 10 m giving 3500
Purity [%] 100 99.7
3500100
Yield [%] 99.7 Enantiomer 1 Enantiomer 2
Warfarin
50
an analytical scale column and translate all the 500 0 0 500 2.0 g
0 10 20 30 0 5 10 15 20 25 30 35
generated data to a larger column packed with [min.] [min.]
0 0
Enantiomer 1 Enantiomer 2
10 m particles. 1 2 3 4 5 6 Purity [%] 99.7 99.5 1 2 3 4 5 6
(70 bar) (70 bar) (70 bar) (70 bar) (100 bar) (100 bar)
Yield [%] 99.4 99.7
(70 bar) (70 bar) (70 bar) (70 bar) (100 bar) (100 bar) Preparative applications
If you plan to scale up the process, we suggest
Cycles of packing (piston pressure) Cycles of packing (piston pressure) Analytical injection Preparative injection
Common conditions Equivalent loading on a
you use an analytical column packed with 10 m
00 particles right from the start. degradation of the material after repeated packings. Actual particle size for 0
0
Chiralcel and Chiralpak is about 3 times larger than that for Kromasil, which 00 = 1.2
explains the difference in initial back pressure (back-pressure is inversely
0
00 proportional to the square of the particle size). 0
00
Easy to Scale up 0
The test was designed to exert greater than normal 00 0
00
Binaphtol
Easy to scale up mechanical stress on the chiral stationary phases, 0
Conditions: Conditions: Conditions: Conditions:
0 5 10 15 20 25
0
5 10 15 20 25
0.1 g
00 and is performed at a packing pressure above the Column size: 4.6 150 mm
Flow rate: 0.5 ml/min
DAC system: NovaSep Pack-n-Sep, 50 mm i.d.
Bed length: 135 mm
Column size: 4.6 150
Flow rate: 0.5 ml/min
DAC system: NovaSep Pack-n-Sep, 50 mm i.d.
Bed length: 132 mm [min.] 0 [min.]
Flow rate: 60 ml/min Flow rate: 60 ml/min Enantiomer 1 Enantiomer 2
maximum 50 bar recommended by the manufac- 500 200 0 500 000 0
Purity [%] 95.4 97.8
Yield [%] 91.7 72.8
0 = 1.4 = 1.3 = 2.9 = 3.0
turer of Chiralcel OD and Chiralpak AD. 00 Rs= 2.6
00
5 0 Rs= 2.4 00 Rs= 9.9 805 0 Rs= 7.9
0 5 10 15 0
50
80 0
50 60
[min.] 600 0 0 0
Analytical injection Preparative injection
Metoprolol
0 5 10 15 20 0 5 10 15 20
Mechanical strength is an important product our detailed quality system, and the final product [min.] [min.]
Enantiomer 1 Enantiomer 2
lifetime parameter. Kromasil AmyCoat and is never released until it has passed our rigorous Purity [%] 100 99.7
Yield [%] 97.9 88.1
Kromasil CelluCoat have a mechanically strong quality control tests. Having all the manufacturing
Common conditions
spherical silica which withstands repeated cycles steps in-house also gives us a strong position in Stationary phase: Kromasil CelluCoat, 10 m Temperature: 25 C
Column size: 4.6 x 250 mm Flow rate: 1 ml/min
HN
3 m - AmyCoat 5 m - AmyCoat 10 m - AmyCoat 3 m - CelluCoat 5 m - CelluCoat 10 m - CelluCoat
NH O O
O
O
O 4.6 Kromasil 3-AmyCoat Kromasil 5-AmyCoat ___
HN
O
4.6 Kromasil 3-CelluCoat Kromasil 5-CelluCoat ___
O HN
x 4.6 x 50 mm 4.6 x 50 mm O O x 4.6 x 50 mm 4.6 x 50 mm
50 mm O 50 mm
O
O * O
O O *
* O O
O O O 4.6 Kromasil 3-AmyCoat Kromasil 5-AmyCoat Kromasil 10-AmyCoat O 4.6 Kromasil 3-CelluCoat Kromasil 5-CelluCoat Kromasil 10-CelluCoat
O O x 4.6 x 150 mm 4.6 x 150 mm 4.6 x 150 mm NH
HN n
x 4.6 x 150 mm 4.6 x 150 mm 4.6 x 150 mm
NH HN O 150 mm O 150 mm
O O
O O
O HN
4.6 Kromasil 3-AmyCoat Kromasil 5-AmyCoat Kromasil 10-AmyCoat 4.6 Kromasil 3-CelluCoat Kromasil 5-CelluCoat Kromasil 10-CelluCoat
NH HN O O
x 4.6 x 250 mm 4.6 x 250 mm 4.6 x 250 mm x 4.6 x 250 mm 4.6 x 250 mm 4.6 x 250 mm
*
250 mm 250 mm
n
10 ___ Kromasil-5-AmyCoat Kromasil-10-AmyCoat 10 ___ Kromasil-5-CelluCoat Kromasil-10-CelluCoat
x 10 x 250 mm 10 x 250 mm x 10 x 250 mm 10 x 250 mm
250 mm 250 mm
tris-(3,5-dimethylphenyl)carbamoyl amylose 21.2 Kromasil 5-AmyCoat Kromasil 10-AmyCoat tris-(3,5-dimethylphenyl)carbamoyl cellulose 21.2 Kromasil 5-CelluCoat Kromasil 10-CelluCoat
x ___ 21.2 x 250 mm 21.2 x 250 mm x ___ 21.2 x 250 mm 21.2 x 250 mm
250 mm 250 mm
Particle sizes Particle sizes
* Other column dimensions available upon request. * Other column dimensions available upon request.
*Due to limited miscibility of methanol in alkanes, ethanol should *Due to limited miscibility of methanol in alkanes, ethanol should
be added as a mediator when exceeding 5% methanol. be added as a mediator when exceeding 5% methanol.
Compatible conditions Further investigations required Compatible conditions Further investigations required