Ira S. Krull

This installation of "Validation Viewpoint" describes how statistically rigorous quality-by-design (QbD) principles can be put into practice to accelerate each phase of liquid chromatography (LC) instrument method development.

While the "Validation Viewpoint" column has focused on conventional and recombinant pharmaceutical products, and at times, bioanalytical methods, we have just begun to think about method validation as it relates to -omics type studies.

HPLC with ELSD continues to grow in popularity as a "quasi- universal" detector. Improvements in ELSD instrument design, including low temperature evaporation, have recently been commercialized...

A very useful construct in engineering and analytical chemistry is the concept of a time-invariant linear system. The properties of the system (as for a mathematical function) are defined by a relationship between the response and the excitation, and ...

To obtain a better understanding of the challenges faced during method development and validation, the authors - in cooperation with LCGC - conducted a survey earlier this year. This column summarizes the results.

This month's "Validation Viewpoint" installment highlights some method validation guidelines used in developing and validating dissolution test procedures.

This installment of "Validation Viewpoint" column addresses, in the hopes of clarifying what the biopharmaceutical industry is required to do today to identify and quantify impurities in their biotech, proteinaceous products.

One issue that has become clear to us throughout courses, workshops, seminars, and various talks on the subject of method validation, is that while many people talk the language, sometimes the individual method validation terms mean different things to different people. While the actual protocols, or experimental details used to measure or evaluate method validation can vary, it's a good idea to have a common understanding of the underlying terms. In this month's installment of "Validation Viewpoint," we have compiled glossary of method validation terms as they pertain to chromatography.

Editor Dave Walsh suggested that current columnists for LCGC might enjoy writing about their experiences in writing their columns and relate how they got into such writings and where it has taken them.

Peptide mapping is one of the preferred techniques for the comprehensive characterization of biopharmaceutical products and is often the analytical method of choice for studying a protein's primary structure.

November 2006. The objective of a formal method transfer is to ensure that the receiving laboratory is well trained, qualified to run the method in question, and gets the same results - within experimental error - as the initiating laboratory. The development and validation of robust methods and strict adherence to well documented standard operating procedures is the best way to ensure the ultimate success of the method. This installment of "Validation Viewpoint" examines the analytical method transfer process, including protocol, documentation, and some possible chromatographic pitfalls to avoid.

After having collected some industry accepted practices for implementing new LC technology, the duo discuss FDA guidance available on the subject with respect to LC, and using some recently introduced LC technology.

The authors define robustness, instroduce a few approaches to designing a robustness study, and discuss data analysis necessary to help ensure successful method implementation and transfer as a part of method validation protocol.

The authors take a look at three recently published documents in the validation literature from groups working to (hopefully!) clear up some of the potential for confusion.

The authors outline the ways in which forced degradation is used to develop a stability-indicating method and examine some of the method development and validation parameters critical to its success.

Second column in a series that reviews impurity method validation guidelines.

This column is the first installment in a two-part series reviewing ICH and FDA impurity method validation guidelines.

This column explores and highlights recently published guidelines for bioanalytical method validation.

Krull and Swartz describe how chromatographers can determine peak purity and identity using new software programs.

This month's "Validation Viewpoint" column examines the reasons behind problems with new drug applications submitted to the U.S. Food and Drug Administration (FDA). Ira Krull and Michael Swartz look at specific problems within analytical methods that raise red flags at the FDA.

Krull and Swartz examine validating cleaning methods for pharmaceutical manufacturing equipment and look at general requirements and specific cleaning procedures, sampling types, and analytical methods.

This month's column describes the ICH, its structure, member bodies, and operating procedures. Editors Krull and Swartz also give readers an update on ICH projects and guidelines.