Um método analítico por cromatografia líquida de alto rendimento com detecção ultravioleta (HPLC-UV) (método A) foi utilizado na determinação simultânea dos valores totais de triacilglicerídeos, diacilglicerídeos, monoacilglicerídeos e ésteres metílicos de ácidos graxos na alcólise de diferentes óleos (algodão, canola, girassol, milho e soja). As análises foram realizadas a 40 °C por 20 min usando gradiente de metanol (MeOH) e 2-propanol-hexano 5:4 (v/v) (PrHex): 100% de MeOH em 0 min, 50% de MeOH e 50% de PrHex em 10 min mantido com eluição isocrática por 10 min. Outro método por HPLC-UV (método B) com eluição isocrática de acetonitrila por 34 min foi utilizado na determinação da composição de ácidos graxos de óleos analisando seus derivados de éster metílico. Os conteúdos foram analisados com satisfatória repetibilidade (desvio padrão relativo, RSD < 3%), linearidade (r 2 > 0,99) e sensibilidade (limite de quantificação). O método B foi comparado com o método oficial cromatográfico gasoso com detecção através de ionização por chama (GC-FID) da American Oil Chemists' Society (AOCS) na determinação de ésteres metílicos de ácidos graxos (FAME) em amostras reais de biodiesel.An analytical method using high performance liquid chromatography with UV detection (HPLC-UV) (method A) was used for simultaneous determination of total amounts of triacylglycerides, diacylglycerides, monoacylglycerides and fatty acid methyl esters in alcoholysis of different oil (cotton, canola, sunflower, corn and soybean) samples. Analyses were carried out at 40 °C for 20 min using a gradient of methanol (MeOH) and 2-propanol-hexane 5:4 (v/v) (PrHex): 100% of MeOH in 0 min, 50% of MeOH and 50% of PrHex in 10 min maintained with isocratic elution for 10 min. Another HPLC-UV method (method B) with acetonitrile isocratic elution for 34 min was used to determine the fatty acid composition of oils analyzing their methyl ester derivatives. Contents were determined with satisfactory repeatability (relative standard deviation, RSD < 3%), linearity (r 2 > 0.99) and sensitivity (limit of quantification). Method B was compared with an official gas chromatographic method with flame ionization detection (GC-FID) from American Oil Chemists' Society (AOCS) in the determination of fatty acid methyl esters (FAME) in biodiesel real samples.Keywords: biodiesel, triacylglycerides, gas chromatography, liquid chromatography, methyl ester
IntroductionThe direct use of fats and oils (mainly composed by triacylglycerides) in diesel engines is problematic and can lead to many problems, such as carbon deposit due to its poor atomization, high viscosity and thickening of lubricating oil as a consequence of its low volatility. 1,2 There are many possible solutions to address the viscosity problem, which are dilution with diesel fuel, microemulsions with short chain alcohols and pyrolysis or transesterification of triacylglycerides. Transesterification is a widespread process used for obtaining biodiesel and involves the catalyzed reaction of triacylglycerides (TAGs) a...