Liquid chromatographic determination of thalidomide in tablets, capsules, and raw materials.
A simple, isocratic liquid chromatographic method for assay of thalidomide in tablets, capsules, and raw materials was developed. The method uses a Nova-Pak octadecylsilane bonded-phase column (150 x 3.9 mm, 4 microns particle size), a mobile phase of acetonitrile-water (15 + 85), a flow rate of 1 mL/min, detection at 237 nm, and phenacetin as internal standard. Phosphoric acid was used in preparation of sample solutions to inhibit thalidomide hydrolysis. Assays ranged from 99.3 to 100.4% in raw materials from 4 manufacturers, from 79.7 to 104.8% in tablets from 7 manufacturers, and from 75.3 to 102.6% in capsules from 4 manufacturers. Assay method precisions for triplicate analyses on 5 days were 0.30% for tablets, 0.22% for capsules, and 0.22% for raw materials. Recovery from simulated tablet formulations was 100%. The method has been used to analyze individual tablets and capsules for determination of content uniformity.
Reepmeyer
J C
JC
U.S. Food and Drug Administration, Division of Drug Analysis, St. Louis, MO 63101, USA.
Cox
D C
DC
D000097:Acetonitriles / Q000737:chemistry; D002214:Capsules / Q000032:analysis*; D002853:Chromatography, Liquid; D007166:Immunosuppressive Agents / Q000032:analysis*; D007917:Leprostatic Agents / Q000032:analysis*; D010316:Particle Size; D010615:Phenacetin / Q000032:analysis; D010756:Phosphoric Acids / Q000737:chemistry; D011358:Product Surveillance, Postmarketing; D012015:Reference Standards; D015203:Reproducibility of Results; D012821:Silanes / Q000737:chemistry; D013056:Spectrophotometry, Ultraviolet; D013607:Tablets / Q000032:analysis*; D013792:Thalidomide / Q000032:analysis*; D014867:Water / Q000737:chemistry
D000097:Acetonitriles; D002214:Capsules; D007166:Immunosuppressive Agents; D007917:Leprostatic Agents; D010756:Phosphoric Acids; D012821:Silanes; D013607:Tablets; D014867:Water; C024779:octadecylsilane; D013792:Thalidomide; C030242:phosphoric acid; D010615:Phenacetin; C032159:acetonitrile