Naslov
Razvoj SPS postupaka za određivanje tragova fenola
(Development of SPS procedures for determination of traces of phenols)

Autori
Vuković, Jadranka ; Yoshimura, Yoshimura ; Matsuoka, Shiro ; Grdinić, Vladimir

Vrsta, podvrsta i kategorija rada
Sažeci sa skupova, sažetak, znanstveni

Skup
Treći hrvatski kongres farmacije s međunarodnim sudjelovanjem

Mjesto i datum
Cavtat, Hrvatska, 27.04.2005. - 30.04.2005

Vrsta sudjelovanja
Poster

Vrsta recenzije
Domaća recenzija

Ključne riječi
SPS; Phenols; Traces

Sažetak
Solid phase spectrophotometric technique was used for development of three simple, sensitive and inexpensive methods for determination of traces of phenols in pharmaceutical preparations: UV-SPS, AAP-SPS and DAR-SPS. The optimum experimental conditions were discussed and metrological characteristics were established. UV-SPS procedure is based on the fixation of the phenol on QAE Sephadex A-25 (40 mg) at pH 11 and posterior measurement of the intrinsic absorbance of the solid phase in a 1-mm cell at 289 nm, without previous derivatization. The method AAP-SPS was performed by sorption and direct absorbance measurement of the product phenol-AAP sorbed on anion-exchanger Dowex 1-X4 (0.2 g) at 495 nm. The procedure DAR-SPS is based on sorption and direct measurement of absorbance of the product phenol-DAR sorbed on anion-exchanger Dowex 1-X2 (0.2 g) at 530 nm. The difference in absorbances at absorption maximum and non-absorption wavelengths was used to give better results for determination of traces of phenol. The sensitivity offered by the procedures was higher by factors of 50 (UV-SPS), 40 (AAP-SPS) and 170 (DAR-SPS) than that provided by respective conventional spectrophotometric methods. The calibration graphs were linear in analyte working range from 6.0-60.0 nmol mL-1 (UV-SPS), 1.0-15.0 nmol mL-1 (AAP-SPS) and 0.2-2.0 nmol mL-1 (DAR-SPS). Limits of detection were 4.20, 0.40 and 0.05 nmol mL-1 for UV-SPS, AAP-SPS and DAR-SPS, respectively. High level of precision (RSD) was obtained: 1.8% (UV-SPS), 3.6% (AAP-SPS) and 1.8% (DAR-SPS). The accuracy was investigated by recovery test adding known amounts of phenol in analyte solution. The recoveries were 99-104% (AAP-SPS) and 98-100% (DAR-SPS). Proposed procedures were used for determination of phenol in salicylic acid as possible impurity according to European Pharmacopoeia. The high speed, ease of use, high level of sensitivity and relative freedom from random contamination by sample handling make these methods ideal for the phenols monitoring in pharmaceutical preparations and offer wider applications.

Izvorni jezik
Engleski

Znanstvena područja
Kemija, Farmacija

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