NMR

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(New page: {{LSApp |name = NMR Sample Prep |image = Dissolution.png |type = Sample Prep |id = Sample Prep |description = NMR Sample Prep }} === Overview === D...)
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=== Overview ===
=== Overview ===
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Dissolution testing of slow-release devices, for example small, polymer coated springs or coils which can be implanted inside the human body and release their drugs over a period of many months or even years. It is applicable to any customer who is developing or manufacturing these devices. This type of testing is a necessary part of the development and or QC process. The objective is to carefully measure the release rate of the drug from the device in-vitro over a period of time. Results are then correlated with data collected in animals.  
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This Twin PAL application involves the preparation of liquid samples and the transfer of them to NMR tubes. The Sample preparation step consists of adding a selected reagent then incubating the sample vial in a heated agitator for a specified length of time. Once the incubation is completed, the sample vial is returned to the sample tray and a consistent volume of the reacted sample is transferred to sealed NMR tubes. It is applicable to any customer who is doing sample prep and the loading of the NMR tubes. This type of sample prep is a necessary part of the NMR process. The objectives are to have every sample treated the same, maximize throughput, and have a consistent sample volume in the NMR tube.  
=== Significant Markets  ===
=== Significant Markets  ===
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This application is ideal for those labs who wish to perform dissolution testing in small vessels. Samples or devices are normally held in vials incubated and shaken for prolonged periods and elution volumes removed and tested periodically. Elements of this application could be applied to labs requiring any type of sample treatments at timed intervals. It also involves storing data about each sample in Excel and protecting the devices from contact with the sampling needle
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This application is ideal for those labs who wish to perform NMR sample prep needing incubation, agitation, and the loading of NMR tubes. Elements of this application could be applied to labs requiring any type of sample prep and maximizing throughput.
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'''What is the sample prep?'''<br/>
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The sample prep procedure is quite simple with the exception of the sample needing to end up in NMR tubes and maximizing throughput. Six Inkwell Reservoirs containing the reagents are available to both PAL’s. The user chooses which reagent they want to add and then the samples are loaded into a standard 6 position agitator for heating and shaking. Since the PAL can not easily move NMR tubes, all of the sample prep was done in 10ml vials with ferrous caps and then transferred to the capped NMR tubes at the end of the process. Despite its simplicity, this process requires the manual preparation of many vials at measured times. It can be a very tedious operation which requires a technician to be in the lab doing a very repetitive process.  It was important that any automation solution allow for the use of caps &septa and maximize throughput to keep up with the existing NMR’s.
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'''What is a Dissolution Testing experiment?'''<br/>
 
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The testing procedure is quite simple. Vials containing the devices are filled with a buffer solution. They are loaded into a special heated and shaking tray. A timer is started. At specified intervals the buffer is removed, a portion of it saved for later analysis, the rest discarded, and the vials replenished with fresh buffer.
 
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Despite its simplicity, this process requires the manual sampling and testing of hundreds of vials at very carefully measured time intervals over a period of days. It is a very tedious operation which requires technicians to be in and out of the lab for hours doing a very mundane job – a classic candidate for automation. It was important that any automation solution did not damage the surface of the devices. There were no existing options to automate this process before the customer approached LEAP.
 
'''LEAPS Approach'''<br/>
'''LEAPS Approach'''<br/>
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The PAL in combination with the LEAP Shell makes a very effective and flexible workstation.<br/>
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The Challenges for LEAP
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We were able to design and provide a solution which met the following challenges from the customer:<br/>
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The Twin PAL in combination with the LEAP Shell makes a very effective and flexible workstation. We were able to design and provide a solution which met the following challenges from the customer:  
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1. Exchanging large volumes of liquid from sealed vials. This requires overcoming vacuum/pressure differentials.<br/>
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1. Throughput. By using a Twin PAL we are able to take advantage of having both PALs preparing samples by sharing all of the reagents, a sample tray and NMR tube rack.  
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2. Protect the slow-release devices from contact and potential damage by the sampling needle. This was achieved using a specially designed vial insert.<br/>
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2. Throughput. Shaking and incubation of a large number of sample vials was accomplished by using two 6 position agitators. LEAP shell provided for maximizing the number of vials in the agitators.
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3. Shaking and incubating a large number of sample vials (>20). We were able to source a suitable heated shaking table for their vials from a third party vendor.<br/>
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3. Filling a capped NMR tube. This was achieved using a specially designed 32 Position NMR tube holder.
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4. Setting up a sampling schedule in the software which would span over several days if necessary. Only possible with the LEAP Shell.<br/>
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4. Provide the flexibility. LEAP Shell easily allowed the changing of the sample batch size and which reagent was to be used by the operator.
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5. Provide the flexibility to change the sample batch size and sampling intervals.<br/>
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6. Record the actual sampling times to a data file – compare actual time with expected time and report a difference.<br/>
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'''Photos'''<br/>
'''Photos'''<br/>
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</gallery>
</gallery>
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'''Keywords:''' Mini Dissolution, Slow release, timed-sampling, Heating, Shaking,
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Keywords:  “NMR”, sample prep, timed-sampling, Heating, Shaking,

Revision as of 16:15, 9 February 2009

NMR Sample Prep
Application Type
  Sample Prep
Application ID
  Sample Prep
Description
  NMR Sample Prep

Overview

This Twin PAL application involves the preparation of liquid samples and the transfer of them to NMR tubes. The Sample preparation step consists of adding a selected reagent then incubating the sample vial in a heated agitator for a specified length of time. Once the incubation is completed, the sample vial is returned to the sample tray and a consistent volume of the reacted sample is transferred to sealed NMR tubes. It is applicable to any customer who is doing sample prep and the loading of the NMR tubes. This type of sample prep is a necessary part of the NMR process. The objectives are to have every sample treated the same, maximize throughput, and have a consistent sample volume in the NMR tube.

Significant Markets

This application is ideal for those labs who wish to perform NMR sample prep needing incubation, agitation, and the loading of NMR tubes. Elements of this application could be applied to labs requiring any type of sample prep and maximizing throughput.

What is the sample prep?
The sample prep procedure is quite simple with the exception of the sample needing to end up in NMR tubes and maximizing throughput. Six Inkwell Reservoirs containing the reagents are available to both PAL’s. The user chooses which reagent they want to add and then the samples are loaded into a standard 6 position agitator for heating and shaking. Since the PAL can not easily move NMR tubes, all of the sample prep was done in 10ml vials with ferrous caps and then transferred to the capped NMR tubes at the end of the process. Despite its simplicity, this process requires the manual preparation of many vials at measured times. It can be a very tedious operation which requires a technician to be in the lab doing a very repetitive process. It was important that any automation solution allow for the use of caps &septa and maximize throughput to keep up with the existing NMR’s.


LEAPS Approach
The Challenges for LEAP The Twin PAL in combination with the LEAP Shell makes a very effective and flexible workstation. We were able to design and provide a solution which met the following challenges from the customer: 1. Throughput. By using a Twin PAL we are able to take advantage of having both PALs preparing samples by sharing all of the reagents, a sample tray and NMR tube rack. 2. Throughput. Shaking and incubation of a large number of sample vials was accomplished by using two 6 position agitators. LEAP shell provided for maximizing the number of vials in the agitators. 3. Filling a capped NMR tube. This was achieved using a specially designed 32 Position NMR tube holder. 4. Provide the flexibility. LEAP Shell easily allowed the changing of the sample batch size and which reagent was to be used by the operator.


Photos

LEAP Dissolution Testing System

Keywords: “NMR”, sample prep, timed-sampling, Heating, Shaking,

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