Laboratory Testing Case Studies

Challenge: Diteba undertook research with the technological objective to develop a suitable procedure that was capable of detecting and quantifying all nine main components in an energy soft drink: caffeine, niacin, vitamin B₆, pantothenic acid, riboflavin, vitamin B₁₂, taurine, glucuronolactone and inositol. The procedure was intended for use in quality control testing and long-term stability testing of energy drinks.

Challenge: To develop and validate a chiral HPLC method capable of monitoring the purity of a Triazole analogue in a novel production process and two other methods: LC/MS/MS for identification of process impurities; and a head space GC method capable of qualitatively and quantitatively monitoring residual organic volatile impurities (OVI) during the manufacturing process.

Challenge: The technological objective of this Diteba project was to develop an in vitro release test method for Lidocaine Ointment USP 5%, a local anesthetic agent that is administered topically.  There were no suitable in vitro release test methods available and the method was necessary as part of the FDA's drug approval process.  The in vitro release test method was to be developed in accordance with the FDA issued guidance covering practice of Scale-up and post approval changes with semi-solids (SUPAC-SS).  A key element in the in vitro release test is to determine if the diffusion release of a drug found in a formulation is the same following the changes made to the formulation.

Challenge: The goal of this work was to investigate the improvement of resolution between all multimer, dimer and monomers in a monoclonal antibody (mAb).  The method was initially developed by the sponsor but failed to demonstrate adequate level of sensitivity and selectivity when used during stability studies.  In addition the resolution between the analytes (monomer, dimer and multimer) was very poor.

Challenge: Typical oligonucleotides used as therapeutics or potential therapeutic compounds are 15 to 30 nucleotides (nt) long. Oligonucleotides <15 nt can be readily resolved by HPLC technology, however the separation of longer sequences are more challenging. Ion-pair reversed-phase (IP-RP) HPLC has been traditionally used for oligonucleotides analysis.  The traditional IP-RPLC eluent system typically uses TEA or TEAA or HFIP and the ion-pairing agent triethylammonium ion and a C18, column at 60^oC. Under such conditions, the column's hydrolytic stability becomes crucial and is important to prevent the potential contribution of the oligonucleotide secondary structure from impacting retention.

The primary technological objective of this project was to develop a more sensitive and reproducible analytical method for detection and quantification of insulin and its metabolites in animal blood serum.  The secondary technological objective was to develop a procedure to monitor drug dose uniformity as well as the in-vitro release rate.

Challenge: The objective of this project was to develop simple, precise, rapid and reproducible analytical methods for the quantification of: a) major Ginsenosides in Panax quinquefolius extract; and b) Flavonols in Ginkgo Biloba extract and use these methods as quality control tools for commercial energy drink products.

Non-nucleoside reverse transcriptase inhibitors (NNRTI's) are antiretroviral drugs used in the treatment of human immunodeficiency virus (HIV).  NNRTI's inhibit reverse transcriptase (RT), an enzyme that controls the replication of the genetic material of HIV.  RT is one of the most popular targets in the field of antiretroviral drug development.  However, separation of all 7 peaks achieved by gradient elution in 45 minutes total run time was unacceptable due to a high sample throughput during stability and quality control programs.  The development of a new rapid and more efficient UPLC^TM analytical method was necessary to overcome the shortcomings of the existing HPLC method.

Challenge: Diteba was commissioned by a sponsor to conduct research for the development of an analytical method for in vitro determination of the release rate of sulfanilamide in topical vaginal cream. The method was developed and based on a modified Franz Diffusion Cells fitted with synthetic membranes.