Validation of an analytical method for quality control of residual solvents (n-hexane and acetone) in D-002: new active ingredient from beeswax.
D-002 is a new natural product consisting of a mixture of aliphatic fatty alcohols, which shows antioxidant and anti-ulcer effects in experimental models. A new validated methodology for determining simultaneously residual n-hexane and acetone in D-002 using the headspace gas chromatography (HS/GC) is described. The very poor solubility of D-002 in most solvents did necessary sample preparations in solid state. Limit test conditions allowed a detection of residual n-hexane and acetone more sensitively than that recommended for such purposes in the general method of the European Pharmacopoeia. Validation assays, applied to both D-002 residual solvents, proved: suitable sensitivity; very high linearity (correlation coefficients > or =0.999, R.S.D. of slopes < or =0.8% and R.S.D. of response factors < or =5% and no biases) and accuracy (average recoveries between 94.7 and 100.1%); and precision was < or =2.1%. The method was found suitable for quality control and stability studies of this new product.
Antolín
Ernesto Méndez
EM
National Center for Scientific Research, Cubanacán, Playa, PO Box 6414, Havana City, Cuba. ernesto.mendez@cnic.edu.cu
Quiñónez
Yaisme Balcinde
YB
Canavaciolo
Víctor González
VG
Cruz
Esperanza Rodríguez
ER
D000096:Acetone / Q000032:analysis*; D002849:Chromatography, Gas; D005233:Fatty Alcohols / Q000032:analysis / Q000592:standards*; D006586:Hexanes / Q000032:analysis*; D011786:Quality Control; D012997:Solvents / Q000032:analysis*
C104511:D 002; D005233:Fatty Alcohols; D006586:Hexanes; D012997:Solvents; D000096:Acetone; C026385:n-hexane