title: Development and validation of a simple high performance liquid chromatography - evaporative light scattering detector method for direct quantification of native cyclodextrins in a cyclization medium.
abstract: A simple HPLC-ELSD method was developed for the separation and quantification of native cyclodextrins. The technique was validated in the presence of two interfering matrices composed of byproducts from the cyclization medium. A fast separation of the compounds was achieved (in <20min) using a NUCLEODUR(®) C18 Pyramid column (150mm×4.6mm; particle size 5μm) at 30°C. The analytes were eluted using a linear gradient of acetonitrile and water containing 1% (v/v) of acetic acid at a flow rate of 0.3mL/min. Validation results showed that the method was accurate (93-110%) and selective. The precision was ≤5.7% for a hydrolyzed starch blank matrix spiked with cyclodextrins, and ≤6.2% for a blank matrix composed of a mixture of dextrin and glucose spiked with cyclodextrins. The limit of quantification was 0.05g/L for alpha- and 0.06g/L for beta- and gamma-cyclodextrins. The new HPLC-ELSD method could accurately quantify the three cyclodextrins directly in a cyclization medium, without pretreatment of the samples.
authors.affiliation: Graduate Program of Chemical Engineering, Federal University of São Carlos, Rod. Washington Luiz, km 235, PO Box 676, 13565-905 São Carlos, SP, Brazil. Electronic address: mayerlenis@gmail.com.
authors.forename: Mayerlenis J
authors.initials: MJ
authors.lastname: Rojas
authors.affiliation: Department of Chemical Engineering, Federal University of São Carlos, Rod. Washington Luiz, km 235, PO Box 676, 13565-905 São Carlos, SP, Brazil. Electronic address: thaiscastral@ufscar.br.
authors.forename: Thaís C
authors.initials: TC
authors.lastname: Castral
authors.affiliation: Graduate Program of Chemical Engineering, Federal University of São Carlos, Rod. Washington Luiz, km 235, PO Box 676, 13565-905 São Carlos, SP, Brazil; Department of Chemical Engineering, Federal University of São Carlos, Rod. Washington Luiz, km 235, PO Box 676, 13565-905 São Carlos, SP, Brazil. Electronic address: raquel@ufscar.br.
authors.forename: Raquel L C
authors.initials: RL
authors.lastname: Giordano
authors.affiliation: Graduate Program of Chemical Engineering, Federal University of São Carlos, Rod. Washington Luiz, km 235, PO Box 676, 13565-905 São Carlos, SP, Brazil; Department of Chemical Engineering, Federal University of São Carlos, Rod. Washington Luiz, km 235, PO Box 676, 13565-905 São Carlos, SP, Brazil. Electronic address: pwtardioli@ufscar.br.
authors.forename: Paulo W
authors.initials: PW
authors.lastname: Tardioli
mesh_terms: D002851:Chromatography, High Pressure Liquid; D003500:Cyclization; D003505:Cyclodextrins / Q000032:analysis*; D008027:Light; D015203:Reproducibility of Results; D012542:Scattering, Radiation; D047392:beta-Cyclodextrins / Q000032:analysis; D047408:gamma-Cyclodextrins / Q000032:analysis
chemical_list: D003505:Cyclodextrins; D047392:beta-Cyclodextrins; D047408:gamma-Cyclodextrins
keywords: Analytical method development; CD quantification; Cyclodextrins; HPLC–ELSD; Validation