Isolation of component materials of aqueous solutions soluble in lipophilic solvents

• US 4,056,468 A
• Filed: 02/25/1975
• Issued: 11/01/1977
• Est. Priority Date: 03/02/1974
• Status: Expired due to Term

• Current Assignee: Merck Patent GmbH (Merck & Co., Inc.)
• Original Assignee: Merck Patent GmbH (Merck & Co., Inc.)
• Inventors: Helger, Roland, Breiter, Joachim
• Primary Examiner(s): Bascomb, Jr., Wilbur L.
• Assistant Examiner(s): Cintins, Ivars
• Application Number:
  US05/553,023
• Time in Patent Office: 980 Days
• Field of Search: 23/230 B, 210/24, 210/31 C, 210/41, 210/31 R, 210/40, 252/449, 252/451
• US Class Current: 210/672
• CPC Class Codes: B01J 20/103 comprising silica
• CPC Class Codes: B01J 20/14 Diatomaceous earth
• CPC Class Codes: B01J 20/28004 Sorbent size or size distribution, e.g. particle size
• CPC Class Codes: B01J 20/28059 being less than 100 m2/g
• CPC Class Codes: B01J 20/28069 Pore volume, e.g. total pore volume, mesopore volume, micropore volume
• CPC Class Codes: B01J 20/281 Sorbents specially adapted for preparative, analytical or investigative chromatography
• CPC Class Codes: B01J 20/283 based on silica
• CPC Class Codes: B01J 20/291 Gel sorbents
• CPC Class Codes: B01J 20/3092 Packing of a container, e.g. packing a cartridge or column of chromatography columns B01D15/206
• CPC Class Codes: B01J 2220/42 Materials comprising a mixture of inorganic materials materials coated or impregnated on a carrier B01J20/32
• CPC Class Codes: B01J 2220/54 Sorbents specially adapted for analytical or investigative chromatography
• CPC Class Codes: G01N 1/405 by adsorption or absorption
• CPC Class Codes: G01N 25/14 by using distillation, extraction, sublimation, condensation, freezing, or crystallisation G01N25/02 takes precedence
• CPC Class Codes: G01N 30/00 Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation G01N3/00, G01N5/00, G01N7/00, G01N9/00, G01N11/00, G01N13/00, G01N15/00, G01N17/00, G01N19/00, G01N21/00, G01N22/00, G01N23/00, G01N24/00, G01N25/00, G01N27/00, G01N29/00 take precedence
• CPC Class Codes: G01N 33/1826 Organic contamination in water
• CPC Class Codes: G01N 33/50 Chemical analysis of biological material, e.g. blood, urine; Testing involving biospecific ligand binding methods; Immunological testing measuring or testing processes involving enzymes or microorganisms, compositions or test papers therefor; processes for forming such compositions, condition responsive control in microbiological or enzymological processes C12Q
• CPC Class Codes: G01N 33/94 involving narcotics or drugs or pharmaceuticals, neurotransmitters or associated receptors
• CPC Class Codes: Y10T 436/104165 Lipid, cholesterol, or triglyceride standard or control
• CPC Class Codes: Y10T 436/107497 Preparation composition [e.g., lysing or precipitation, etc.]
• CPC Class Codes: Y10T 436/108331 Preservative, buffer, anticoagulant or diluent
• CPC Class Codes: Y10T 436/255 : including use of a solid sorbent, semipermeable membrane, or liquid extraction

Abstract

Process for the isolation of component materials of aqueous solutions by adsorption of the aqueous solutions on concentration agents based on silica gel and/or kieselguhr and subsequent extraction of the component materials with lipophilic solvents, which employs as concentration agents flowable silica gels and/or kieselguhrs with an average particle size of 0.05 to 1.0 mm., an average pore volume of 0.2 to 3 ml./g., and a specific surface of 0.2 to 50 m² /g.

Claims

1. In a process for the isolation of lipophilic solvent-soluble components from an aqueous solution containing lipophilic components comprising contacting the aqueous solution with one or both of a silica gel-based or kieselguhr-based concentration agent to absorb said aqueous solution therein and subsequently extracting substantially only the lipophilic solvent-soluble components from the aqueous solution absorbed in the concentration agent with a lipophilic solvent, the improvement which comprises employing as the concentration agent a flowable silica gel of kieselguhr or a mixture thereof, having an average particle size of 0.05 to 1.0 mm., an average pore volume of 0.2 to 3 ml./g. and a specific surface to 0.2 to 50 m² /g., and said extracting is conducted without substantial simultaneous desorption of the water of said absorbed aqueous solution, said lipophilic solvent-soluble components being at least one analgesic, sedative, hypnotic, anti-epileptic, psychopharmaceutical, sympathicomimetic, anti-histamine, narcotic, alkaloid, antibiotic, lipid, triglyceride, fatty acid, steroid or porphyrin.

2. A process according to claim 1, wherein the concentration agent is a silica gel with an average particle size of 0.15 to 0.4 mm., an average pore volume of 0.5 to 1.7 ml./g. and a specific surface of 0.3 to 20 m² /g.

3. A process according to claim 2 wherein the specific surface of the silica gel is not more than 0.8 m² /g.

4. A process according to claim 2 wherein said silica gel has a specific surface of 0.8 m² /g., an average pore diameter of 40,000 angstroms and a pore volume of 0.7 ml./g.

5. A process according to claim 1, wherein the concentration agent is a kieselguhr with an average particle size of 0.15 to 0.4 mm., an average pore volume of 0.5 to 1.7 ml./g. and a specific surface of 0.5 to 5 m² /g.

6. A process according to claim 1, wherein the aqueous solution is a body fluid.

7. A process according to claim 6, wherein the body fluid is a sample of urine.

8. A process according to claim 1, wherein the weight ratio of aqueous solution to concentration agent is from 1:

0.4 to 1;

1.25 for kieselguhr and from 1;

0.9 to 1;

1.7 for silica gel.

9. A process according to claim 1, wherein the solvent is a water immiscible organic solvent or mixtures thereof or is a mixture of water immiscible and water miscible organic solvents.

10. A process according to claim 9, wherein the water immiscible solvent is a chlorinated alkane and the water miscible solvent is isopropanol.

11. A process according to claim 1, wherein a measured amount of the concentration agent is packaged in a single-use container adapted to store the concentration agent with the aqueous solution adsorbed thereon prior to extraction of the lipophilic-soluble components from the aqueous solution absorbed in the concentration agent with a lipophilic solvent.