Preparation and characterization of formulations in a high throughput mode

• US 7,501,094 B2
• Filed: 09/15/2003
• Issued: 03/10/2009
• Est. Priority Date: 09/15/2003
• Status: Active Grant

• Current Assignee: Syngenta Limited (China National Chemical Corporation)
• Original Assignee: Syngenta Limited (China National Chemical Corporation)
• Inventors: Nettleton-Hammond, John Henry, Lukkari, Ingrid Gunborg, Bysouth, Stephen Robert, Bohara, Amrish, Landham, Rowena Roshanthi, Bergstrom, Karin Ingegard, Hite, Sidney Wilson III
• Primary Examiner(s): Gordon; Brian R.
• Application Number:
  US10/662,142
• Publication Number:
  US 20050058574A1
• Time in Patent Office: 2,003 Days
• Field of Search: 422/100, 422 63- 67, 422/68.1
• US Class Current: 422/63
• CPC Class Codes: B01J 2219/00308 interchangeably mounted in racks or blocks
• CPC Class Codes: B01J 2219/00315 Microtiter plates
• CPC Class Codes: B01J 2219/00322 the individual reactor vessels being arranged serially in stacks
• CPC Class Codes: B01J 2219/00364 Pipettes
• CPC Class Codes: B01J 2219/00479 Means for mixing reactants or products in the reaction vessels
• CPC Class Codes: B01J 2219/00549 2-dimensional
• CPC Class Codes: B01J 2219/00691 using robots
• CPC Class Codes: B01J 2219/00704 integrated with the reactor apparatus
• CPC Class Codes: B01J 2219/00756 Compositions, e.g. coatings, crystals, formulations
• CPC Class Codes: C40B 70/00 Tags or labels specially adapted for combinatorial chemistry or libraries, e.g. fluorescent tags or bar codes
• CPC Class Codes: G01N 11/00 Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties
• CPC Class Codes: G01N 15/0227 using imaging; using holography
• CPC Class Codes: G01N 15/0272 with screening; with classification by filtering B01D takes precedence
• CPC Class Codes: G01N 2035/00198 Dissolution analysers
• CPC Class Codes: G01N 2035/00217 involving measurement of weight
• CPC Class Codes: G01N 2035/00524 Mixing by agitating sample carrier
• CPC Class Codes: G01N 2035/00564 Handling or washing solid phase elements, e.g. beads
• CPC Class Codes: G01N 2035/00752 bar codes
• CPC Class Codes: G01N 2035/0405 manipulating closing or opening means, e.g. stoppers, screw caps, lids or covers
• CPC Class Codes: G01N 2035/103 using disposable tips
• CPC Class Codes: G01N 2035/1032 : Dilution or aliquotting
• CPC Class Codes: G01N 35/0099 : comprising robots or similar manipulators robots per se B25J
• CPC Class Codes: Y10T 436/2575 : Volumetric liquid transfer

Abstract

The invention is an automated robotic system for the production and testing of formulations at a very high throughput. It is an integrated system of hardware and software capable of preparing and evaluating hundreds of emulsions per day. The system can formulate aqueous solutions (SL), oil in water emulsions (EW), suspo-emulsions (SE), micro capsule suspensions (CS), micro-emulsions (ME), and suspension concentrates (SC) at the 1 ml to 25 ml scale. The system can process emulsions rapidly in an automated way and enable very flexible formulation recipes to be introduced.

The system allows chemists to generate experimental samples of varying recipe and method to be conducted in parallel with projected throughput of up to 1200 formulations processed and characterized per day. Materials and consumables can be distributed from storage storage systems to the work stations where dispensing of ingredients in various states can be performed, including solids, liquids, gels, pastes, suspensions and waxes. The emulsions formed can be characterized using methods including phase diagnosis, turbidity analysis, viscosity and particle sizing using automated test equipment. An integrated module can also perform Tank Mix Compatibility testing in high throughput mode. The modular system allows future processes and tests to be added, either to a station, or as a new station. The software capability includes tracking of processes from start to finish and the integration of analytical data with the as-designed and as-formulated experimental results.

Claims

1. A modular robotic system comprising:

a rack and vial storage system storing therein a plurality of racks and vials;

a consumables storage system storing materials;

a first, second and third location;

a first robotic arm for transferring said vials from said first location to said second location, or for transferring said racks from said first location to said second location;

a dispensing, pipetting or characterization station or solid dispensing station for dispensing active ingredients, water, or additives to said vials to yield a formulation,

wherein said first robotic arm transfers materials from said consumables storage system to said dispensing, pipetting, or characterization station or to said solid dispensing station;

a mixing or homogenizing station for mixing or homogenizing said, formulation to yield a mixture;

a phase stability station for phase analysis of said mixture;

optionally a liquids, suspensions, gels or meltables station and

optionally a capping, decapping, bar-code reading or cap-supply station;

wherein said first location is

said rack and vial storage system,

said dispensing, pipetting or characterization station,

said mixing or homogenizing station, or

said phase stability station; and

wherein said second location

said rack and vial storage system,

said dispensing, pipetting or characterization station,

said mixing, or

said phase stability station; and

a flexible second robotic arm, wherein said flexible second robotic arm transfers said racks or said vials from said first robotic arm to said third location upon said modular robotic system where said third location is said capping or decapping or bar-code reading or cap-supply station;

said rack and vial storage system,

said dispensing, pipetting or characterization station,

said mixing or homogenizing station,

said phase stability station,

said solid dispensing station or

said liquids, suspensions, gels or meltables station.

2. The modular robotic system of claim 1, further comprising a comminution station for grinding solid particles, wherein said solid particles are active ingredients or additives and wherein said flexible second robotic arm transfers said racks from said first robotic arm to said comminution station.

3. The modular robotic system of claim 1, wherein said racks each hold up to six said vials, wherein said racks are each bar coded and wherein said vials are each bar coded;

wherein said materials are selected from the group consisting of said vials, pipette tips, said active ingredients and said additives; and

wherein said dispensing, pipetting, or characterization station further comprises;

a waste station, wherein fluid may be pumped to waste; and

a tool head, wherein said tool head is fitted with at least one item selected from the group of items consisting of rack gripper, plate gripper, vial gripper, filter gripper, cap gripper, pipettor and dispense needle.

4. A modular robotic system comprising:

a rack and vial storage system storing therein a plurality of racks and vials;

a consumables storage system storing materials;

afirst, second, and third location;

a first robotic arm for transferring said vials from said first location to a said second, or for transferring said racks from said first location to said second location;

a dispensing, pipetting or characterization station for dispensing active ingredients, water or additives to said vials;

a solid dispensing station for dispensing solids by weight into said vials, wherein said solids are active ingredients or additives;

a liquids, suspensions, gels or meltables station for dispensing viscous fluid, gels, pastes or meltables, wherein said high viscous fluids, said gels, paste and meltables are active ingredients or additives;

wherein said combination of said active ingredients, water, and additives from said dispensing, pipetting or characterization station, said solid dispensing station or said liquids, suspensions, gels or meltables station yields a formulation;

a mixing or homogenizing station for mixing or homogenizing said formulation to yield a mixture; and

a phase stability station for phase analysis of said mixture;

a flexible robotic arm station, including a flexible second robotic arm that transfers said racks from said first robotic arm to said third location upon said modular robotic system; and

a comminution station for grinding solid particles;

wherein said first location is;

said rack and vial storage system;

said dispensing, pipetting or characterization station

said mixing or homogenizing station;

said phase stability station;

said solid dispensing station;

said liquids, suspensions, gels;

or meltables station;

or

said comminution station;

wherein said second location is;

said rack and vial storage system;

said dispensing, pipetting or characterization station;

said mixing or homogenizing station;

said phase stability station;

said solid dispensing station;

said liquids, suspensions, gels, or meltables station;

said flexible arm station;

or

said comminution station; and

wherein said third location is;

said rack and vial storage system;

said dispensing, pipetting or characterization station;

said mixing station;

said phase stability station;

said solid dispensing station;

said liquids, suspensions, gels or meltables station;

or

said comminution station.

5. The modular robotic system of claim 4,

wherein said racks each holds up to six said vials, wherein said racks are each bar coded and,

wherein said vials are each bar coded;

wherein said materials are selected from the group consisting of said vials, pipette tips, said active ingredients and said additives; and

wherein said dispensing, pipetting or characterization station further comprises;

a waste station, wherein fluid may be pumped to waste;

a tool head, wherein said tool head is fitted with at least one item selected from the group of items consisting of;

rack gripper, plate gripper, vial gripper, filter gripper, cap gripper, pipettor and dispense needle; and

a deck;

wherein said deck is mounted with at least one device selected from the group of devices consisting of;

bar code reader, decapper, cap source, orbital shaker, tank mix testing unit, injection port, dilution port, filtration device, particle size detector, viscometer, waste station, bead collector, photography system, trash collection chute and particle microscopy system.

6. The modular robotic system of claim 4,

wherein each said rack includes an identifying bar code;

that is read by said first robotic arm.

7. The modular robotic system of claim 5,

wherein said liquids, suspensions, gels or meltables station further comprises:

a second tool head, wherein said second tool head is fitted with at least one item selected from the group of items consisting of rack gripper, plate gripper, vial gripper, gel dispensor gripper, cap gripper, pipettor and vacuum canula; and

a second deck;

wherein said second deck is mounted with at least one device selected from the group of devices consisting of;

movable gel dispensor, comminuting bead source, bar code reader, decapper, orbital shaker, heated block, mass balance and trash collection chute.

8. The modular robotic system of claim 7, further comprising:

a second dispensing, pipetting or characterization station, wherein said second dispensing, pipetting or characterization station further comprises a third deck and a third tool head, wherein said third tool head is fitted with at least one item selected from the group of items consisting of rack gripper, plate gripper, vial gripper, gel dispensor gripper, cap gripper, pipettor and dispense needle; and

wherein said third deck is mounted with at least one device selected from the group of devices consisting of;

bar code reader, capper, decapper, caps source, balance, injection port, drain waste station, gel dispenser, orbital shaker and heated block.

9. The modular robotic system of claim 8, further comprising:

an off deck, wherein said off deck is mounted with at least one device selected from the list of devices consisting of second particle size detector, flush system, second viscometer and second particle microscopy system.