A fast, simple and inexpensive procedure is described for the determination of gossypol in cottonseed meal. The procedure is based on a flow injection analysis system and a complexation reaction with spectrophotometric detection at 620 nm. A fluidized bed column was used to implement the on line that was coupled to the extraction flow system in order to analyze the solid samples directly. A linear response was observed from 0.96 to 3.85 mmol L -1 , and the detection limit, the coefficient of variation and the sampling rate were estimated at 100 µmol L -1 (99.7% confidence level), 1.90% (n = 20) and 30 h -1 , respectively. The reagent consumption was 1.08 mg of Fe(NO 3 ) 3 , with a volume of 20 mL of effluent per determination. Analyses of the results of commercial samples were consistent with through the official procedure of detoxification of cottonseed meal as described by American Oil Chemists' Society (AOCS) at the 95% confidence level.
Keywords: gossypol, flow analysis, spectrophotometric detection
IntroductionCottonseed meal is obtained in the oil extraction process. It is high in protein, fiber and minerals and can be used as a fertilizer and animal feed. However, its use is limited by the presence of the polyphenolic yellow compound known as gossypol.1 Gossypol (2,2'-bis(8-formyl-1,6,7-trihydroxy-5-isopropyl-3-methylnaphthalene) is a toxic pigment that occurs in various parts of cotton plants. 2 It is undesirable for different animal species, especially for poultry and swine. 3 Several procedures have been described in the literature for the analysis of gossypol, including procedures based on high performance liquid chromatography (HPLC), 4,5 enzyme-linked immunosorbent assay 6 and Fourier transform infrared spectroscopy (FTIR). 7 The spectrophotometric determination of gossypol can be performed using 3-amino-1-propanol and its subsequent complexation with iron(III), forming a green-colored complex with maximum absorption at 620 nm. To extract the analyte from the cottonseeds, 80 mL of hexane-isopropyl alcohol is used per determination.2 Another procedure is based on secondderivative ultraviolet spectrophotometry and it involves the extraction of free gossypol using aqueous acetone, hydrolysis of the soluble-bound forms with hydrochloric acid and the partitioning of the pure compound into chloroform. The proposed method showed good precision (4.0%), but a large amount of organic solvents was used (50 mL acetone and 50 mL chloroform) and a lot of time was spent (2 h) on each sample.8 These drawbacks hinder the use of these procedures for routine analysis.Flow-injection systems (FIA) have been employed especially for the mechanization of analytical procedures in order to minimize the analyst intervention and enhance the number of samples processed by time and improving precision. In the preparation of samples, FIA can be used to minimize risks of sample contamination and amounts of organic solvents, as well as reduce costs of analysis. These systems also show great potential for the development of greener ...