|Articles|January 1, 2001

LCGC North America

  • LCGC North America-01-01-2001
  • Volume 19
  • Issue 1

Analytical Procedures and Method Validation: Highlights of the FDA's Draft Guidance

The FDA recently updated its 1987 guidelines for submitting samples and analytical data for method validation — a document that affects all analytical chemists working in the pharmacrutical industry. This article highlights the agency's recommendations of how to report and validate analytical data in all new drug applications.


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Chromatography Detects Toxins in Tea Samples
High-performance liquid chromatography-tandem mass spectroscopy (HPLC–MS/MS) chromatography reveals pyrrolizidine alkaloids (PA)/pyrrolizidine alkaloid N-oxides (PANO) toxin risks in 63 tea samples.
Figure 2. Split injection used to measure triplicate test of MTBE, hexane, o-xylene, and 1-methylnaphthalene comparing different solvents (methanol, methylene chloride) and column insertion distances starting with 0.5 mm, 5.0 mm, 10.0 mm, 15 mm, and 20.0 mm. Methanol had the best performance at the 5.0 mm insertion distance and methylene chloride looked slightly better at the 0.5 mm. We would still recommend not going below the 5.0 mm manufacturer recommended insertion distance.
Revisiting insertion distance for methanol and methylene chloride in GC analysis and confirming that insertion depth strongly affects response and reproducibility.