Validation of a gas chromatographic method for determining fatty acids that compose D003 in 10 mg film-coated tablets.
D003 is a new product composed of a mixture of aliphatic fatty acids (C(24:0) to C(36:0)), which shows antiplatelet, antithrombotic, antioxidant, and cholesterol-lowering effects in experimental models and human beings. A gas chromatographic method using a DB-5 wide-bore column and 1-nonadecanoic acid as internal standard was developed and validated in order to determine D003 in 10 mg film-coated tablets. The acids were analysed as methyl esters derivatives, prepared using 5% aqueous HCl-methanol. Developed method was specific for the active principle, even when samples were subjected to stress conditions. Good linearity (correlation coefficient > 0.99) and accuracy (total average recovery = 100.29%) were proven over a range 50-150% of the nominal concentration. Within-day and intermediate precisions at the nominal dose (100%) were < 1.5%. Robustness was examined through an intralaboratory study, quantification and resolution were only affected by the injection volume increase and no other of the 7 operational changes evaluated affected the results. The method was suitable for quality control and stability studies of these tablets.
Antolín
Ernesto Méndez
EM
Center of Natural Products, National Center for Scientific Research, Cubanacán, Playa, PO Box 6414, Havana City, Cuba. clinica@enet.cu
Marrero Delange
David
D
González Canavaciolo
Víctor
V
Tejeda Díaz
Yanet
Y
Sierra Pérez
Roxana
R
Cora Medina
Miriam
M
D000818:Animals; D000924:Anticholesteremic Agents / Q000032:analysis* / Q000737:chemistry; D002849:Chromatography, Gas / Q000379:methods* / Q000592:standards; D004355:Drug Stability; D005227:Fatty Acids / Q000032:analysis* / Q000737:chemistry; D006801:Humans; D011786:Quality Control; D015203:Reproducibility of Results; D013608:Tablets, Enteric-Coated / Q000032:analysis* / Q000737:chemistry
D000924:Anticholesteremic Agents; C478823:D003 preparation; D005227:Fatty Acids; D013608:Tablets, Enteric-Coated