« ALOX FOR CHROMATOGRAPHY AND PURIFICATION PROCESSES »

For Chromatography and Purification Processes

Aluminium Oxide is one of the most versatile sorbents for preparative chromatography. Due to its amphoteric character, Aluminium Oxides can be used in specifically defined pH ranges.

CAMAG manufactures the various types of Aluminium Oxide, which are used in the following processes:

Pilot Plant preparation column chromatography Genzyme Pharmaceuticals
Pilot Plant preparation column chromatography Genzyme Pharmaceuticals

Preparative Column Chromatography

is a widely used technique to separate and purify API’s (Active Pharmaceutical Ingredient) from lab scale to pilot plant and up to production scale in large columns under hydrostatic or low pressure. Since the Aluminium Oxides are of a wide particle size range, packing techniques must insure that segregation does not occur. This is best accomplished by dry packing, then equilibrating the alumina with the solvent to be used for the separation. If wet packing is done, it must be done with a thick mud-like slurry.

Flash Chromatography

is a rapid form of preparative column chromatography. Prep LC based upon «an air pressure driven hybrid of medium and short column chromatography optimized for rapid separation». Flash chromatography is typically used when the differences on TLC are greater than 0.15 Rf units. Flash Chromatography is a simple and economical approach to Prep LC.

Selective filtration

is done by feeding the contaminated solvent extract through a short bed of Aluminium Oxide in large column systems which are run under vacuum, hydrostatic or gas pressure. Two typical modes are found: ‹Frontal Elution› or ‹Solid Phase Extraction›. ‹Frontal Elution› of the extract is commonly used when the extract is complex and/or colored. The extract is fed through a bed of Aluminium Oxide while the decolorized product is collected. Solid Phase Extraction of the mixture is preferred when the product is highly diluted. The product is selectively bound to Aluminium Oxide and eluted in a small volume after saturation of the matrix.

Application

Recommended type of Aluminium Oxide

Alkaloids: Basic, medium activity
Isolation, of ergot-, opium-, rauwolfia-, and other alkaloids

Antibiotics: Neutral
Isolation, purification

Essential Oils: Basic, Neutral
Removal of terpenes

Plant Extraction: Basic, Neutral, Acid
Isolation of active substances


Dehydration of organic solvents: Basic, highly active

Enzymes: Neutral
Purification

Glycosides: Neutral
Isolation of digitalis-, strophantus-glycosides,etc.

Removal of Peroxides: Basic, highly active
From organic solvents


Hormones: Neutral
Isolation and purification of ketosteroids from neutral materials

Purification of organic solvents: Basic, highly active
For technical purposes

Oils: Basic
Clarification of fatty oils, separation of fatty acids


Method Development

Thin-layer chromatography (TLC) is a convenient and fast technique that most of the time provides complete separation of fairly complex mixtures. Any sample type that has been successfully separated by TLC on silica or alumina plates can be separated by means of liquid / solid chromatography. Mobile phase optimization using TLC can easily be carried out using CAMAG HPTLC Variosystem. This Brockmann Activity Normally Aluminium Oxide is used with activity I. The relative humidity of Aluminium Oxide is highly responsible for the chromatographic result. In the state of equilibration the rel. humidity corresponds with the activity. The correlation between rel. humidity and activity acc. to Brockmann is shown in the table. system allows a sample with six different mobile phases to be tested in parallel on one plate within a very short period. Taking some basic rules into account, the mobile phase composition established by means of TLC can be used directly for preparative chromatographic applications.

CAMAG's expertise

CAMAG has manufactured Aluminium Oxide since 1959.

The product, widely used in the pharmaceutical and chemical industries in purification processes is of excellent quality due to the fact that CAMAG has well-trained employees, has a reliable supplier of the raw material, and a standardized manufacturing process.


Testing of Aluminium Oxide

CAMAG tests a number of parameter such as pH, water content, as well as particle size, to assure quality and specification of Aluminium Oxide. pH is measured of a 10% aqueous solution in suspension. Water content is measured in a micro wave analyzer. Particle size is measured in a laser-particle-sizer.


SQS Certificate ISO 9001-2000

CAMAG has a comprehensive Quality System according to ISO 9001:2000. The quality assurance starts at product development, proceeds through quality control of all purchases, and covers all stages of production including final inspection.

The CAMAG laboratory works in accordance with ISO 17025 standard.

Product Data

Particle Size distribution

  max. 2% 

  > 160 μm  

  ~ 95% 

  40-160 μm 

  max. 5% 

  < 40 μm 

 


Brockmann Activity

Normally Aluminium Oxide is used with activity I. The relative humidity of Aluminium Oxide is highly responsible for the chromatographic result. In the state of equilibration the rel. humidity corresponds with the activity. The correlation between rel. humidity and activity acc. to Brockmann is shown in the table.

 Relative Humidity 
  % Water Added 
  Activ. Grade (Brockmann) 
  Rf of Dye* 
0% 0 I 0.15
3.4% 3 II 0.22
7.5% 6 III 0.33
20% 10 IV 0.44
40% 15 V 0.65

* Dye = p-dimethylaminoazobenzene (dimethylyellow, butter yellow (C. I. 11020))


Properties of Standardized Aluminium Oxides

 

 

Catalogue No.

 

 
5016-A basic

507-C
neutral

 506-C
weakly acidic

504-C
Acidic


4516-A
basic**

 

 

CAS No.

1344-28-1

Packing sizes

1kg, 5kg, 25 kg, 50 kg

pH (10% aq. suspension)

9.5 ± 1.0

7.0 ± 0.5

6.0 ± 0.5

4.5 ± 0.5

Mean pore diameter [A]

60

Pore volume [ml/g]

~  0.25

Bulk density [g/L]

~  920

Specific surface area Approx.

150 m2 /g ± 10%

Cl' [mval/g]

0

≈ 0.03 mval/g

≈ 0.06 mval/g

≈ 0.14 mval/g

Na2O [%]

< 0.4%

Fe2O3 [%]

< 0.03%

SiO2 [%]

< 0.03%

Appearance

powder, no lumps

Color

white, off white

** Sligthly higher surface area than 5016-A

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