Distributed Pharmaceutical Analysis Lab

The Distributed Pharmaceutical Analysis Lab (DPAL) provides high quality, validated  chemical analysis of pharmaceutical samples from partners in the developing world.  This collaboration with Chemists Without Borders uses analytical resources at academic institutions in the US to perform characterization of suspect medications that have been collected and screened in Kenya, Uganda, Tanzania, India, Nepal, or Malawi.  

Who is participating in DPAL?  (click on arrow to see list of institutions)

How it works:

When you join DPAL, we will open a project folder for your institution at the Open Science Framework DPAL site. The project site hosts the most current methodology for analyzing different drugs and Excel spreadsheets for entering data.  Your students will upload their data and snapshots of their lab notebooks to your institution's folder.  You can register your data at any time, which creates an unique DOI leading to a web archive showing the data at the point you write a report or prepare a publication/presentation. 

DPAL provides standard HPLC methods and procedures and standard samples for validating the methods on your instruments. After you find your system's linear range for pure API, we will ship you expired samples to test matrix recovery. Once you have shown that your system and sample preparation method is suitable for the analysis of the target pharmaceutical, we will ship you samples collected in Kenya.  You analyze the samples and perform the QC checks and return the analytical data and your conclusions to DPAL.  Suspicious samples undergo additional analysis at UND and then we write a report to alert the appropriate country medical regulatory authorities and sometimes, the WHO.  

System validation and analysis of the samples can be incorporated into undergraduate research, a chemistry club activity, or into formal coursework such as an instrumental analysis or analytical chemistry lab.  Each participating lab follows these steps:

  1. Find the linear range and other analytical metrics of your system using pure API samples
  2. Test sample preparation by doing a matrix spike/recovery
  3. Prepare and analyze 20-40 samples
  4. Report data

Download the Methodology Manual (August 2016 update!  New, Improved!)

hplc_methodology_manual_8.5.2016.pdf

This manual is a work in progress.   Questions and comments are welcome.  The first sections describe how to choose and validate HPLC assays;  suggested assay conditions for several antibiotics are included at the end of the manual.  Other assays may be found in pharmacopeia monographs, such as the WHO's International Pharmacopoeia.  

LC Data Processing Templates for Excel are available on the Open Science Framework project site;  when you become a DPAL participant, you'll get access to these.   

How to get started:

A faculty member must be formally responsible for managing the project and taking custody of the samples. Contact Prof. Marya Lieberman to discuss this process and learn how to register for the OSF project site.  

A good starting point is to download the methodology manual (use the link above) and check the availability of a suitable HPLC system and columns;  most C18 columns are suitable for amoxicillin or ampicillin analysis. Depending on your location, technical assistance with repairing or testing HPLCs may be available through Chemists without Borders.

Why we're doing this

The suspicious sample of amoxicillin/clavulanate below was discovered during an HPLC training session for summer undergraduate researcher Rebecca Ryan.  Clavulanate is a potentiating agent that enables amoxicillin to kill resistant bacteria.  Thanks to the efforts of undergraduate researchers at DPAL, this sample was reported to the Kenyan medical regulatory authorities and the World Health Organization RapidAlert system in 2014;  the product is currently under quarantine in Kenya.  

HPLC traces of suspicious and normal samples of amoxicillin/clavulanate capsules collected in Western Kenya in 2013

 

 

 

 

 

 

 

 

Samples  

We have hundreds of samples of amoxicillin, ampicillin, amoxicillin-clavulanic acid tablets, azithromycin, ciprofloxacin and acetaminophen tablets  purchased by secret shoppers from 239 registered and unregistered pharmacies in 11 towns in western Kenya.

Smaller numbers of samples are also available of other antibiotics, TB medications, antimalarials,worming medications, pharmaceuticals for chronic conditions like diabetes, and veterinary medicines.