Automating HPLC and GC Analytical Method Validation

The chromatographic analytical method validation process involves a series of activities that are currently conducted in separate “technology islands” using tools that exist for each activity.This article describes a software program that provides an overarching automation technology for analytical method validation and brings together the individual activities under one integrated-technology platform that is adapted to multiple instruments and data systems.

These activi ties often are captu red in company stand ard opera ting procedu re (SOP) documents that usu a lly incorpora te US Food and Drug Administrati on and In ternational Conference on Harmonization (ICH) requirements and guida nces(1–3).Met h od validati on SOP doc u m ents de s c ri be all aspects of the method validation work for each experiment type (e.g., accuracy and linearity) within a framework of three general exec uti on sequ en ce steps: ex peri m ental plan, i n s trumental procedures, and analysis and reporting of results. The indivi dual el em ents within these three gen eral steps are det a i l ed in the following paragraphs.

Step 1: experimental plan. An ex peri m ental plan should speci fy a n a lyte concen tra ti ons, i n s trument para m eters ,and envi ronm ental para m eters .The plan also should inclu de the nu m ber of levels per variable, the number of prepara ti on replicates per samp le, and the nu m ber of i n j ecti ons per prep a ra ti on rep l i c a te .An integra ti on of standards, i n clu s i on of s ys tem su i t a bi l i ty injecti on s , and the accept a n ce criteria also are part of the plan.

 Step 2: instrumental procedures.The instru m ental procedu re s s tep invo lves making the requ i red transform a ti ons of the experi m ent plan into the native file or data formats of the instrum en t’s con trolling ch rom a togra phy data sys tem (CDS) sof tw are (con s tru cti on of sample sets and met h od sets or sequ ence and met h ods files). In ad d i ti on , the fo ll owing are specified: the nu m ber of injecti ons (rows), the specific type of each injecti on (e.g., sample or standard ) , and the requ i red modificati ons to the analytical method (robustness).

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