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2014, vol. 64, br. 3, str. 271-284
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Razvoj i validacija RP-HPLC metode za analizu višekomponentnog sirupa za kašalj
Development and validation of RP-HPLC method for analysis of multicomponent cough-cold syrup formulation
Univerzitet u Beogradu, Farmaceutski fakultet, Institut za farmaceutsku hemiju i analitiku lekova, Srbija
e-adresa: blucic@pharmacy.bg.ac.rs
Projekat: Razvoj molekula sa antiinflamatornim i kardioproaktivnim dejstvom: strukturne modifikacije, modelovanje, fizičkohemijska karakterizacija i formulaciona ispitivanja (MPNTR - 172041)
Keywords: RP-HPLC; validation of the method; cough-cold syrup formulation
Sažetak
U ovom radu opisana je brza, efikasna, ekonomična reverzno fazna HPLC metoda za identifikaciju i određivanje doksilamin-sukcinata, efedrin-hidrohlorida, dekstrometorfanhidrobromida, paracetamola kao aktivnih komponenti i natrijum-benzoata kao konzervansa u sirupu za kašalj. Razdvajanje komponenata, njihova identifikacija i određivanje postignuto je na C18 stacionarnoj fazi (XTerraTM RP 18, Waters (150 mm x 4,6 mm, 5 μm veličine čestica) uz gradijentno eluiranje sa mobilnom fazom koju čine voda (čiji je pH podešen na 2,5 sa ortofosfornom kiselinom) i acetonitril kao organski rastvarač. Za detekciju ispitivanih jedinjenja korišćen je UV/VIS detektor podešen na 210 nm (doksilamin sukcinata, efedrin-hidrohlorida, dekstrometorfan-hidrobromida i natrijum-benzoata) tj. 270 nm (paracetamol). Kako je definisana metoda namenjena za identifikaciju i određivanje aktivnih supstanci i konzervansa u sirupu za kašalj, od parametara validacije ispitani su: selektivnost/specifičnost, linearnost, tačnost i preciznost. Svaki od parametara je statistički potvrđen. Dobijene vrednosti statističkih parametara (r³ 0,999, CV£ 2 % i Recovery od 98 % - 102 %) ukazuju da je definisana RP- HPLC metoda pogodna za identifikaciju i određivanje doksilamin-sukcinata, efedrinhidrohlorida, dekstrometorfan-hidrobromida, paracetamola i natrijum-benzoata u sirupu za kašalj.
Abstract
In this study a reversed phase HPLC method for rapid and simultaneous identification and quantification of doxylamine succinate, ephedrine sulfate, dextrometorphane hydrobromide, paracetamole and sodium benzoate in cough-cold syrup formulation was described. Separation was carried out on XTerraTM RP 18, Waters (150 mm x 4.6 mm column, 5 μm particle size). For the analysis of investigated substances gradient elution was used employing water, pH adjusted at 2.5 with 85 % ortophosphoric acid as the mobile phase A and acetonitrile as the mobile phase B. Detection was carried out by UV absorbance at 210 nm for doxylamine succinate, ephedrine sulfate, dextromethorphane hydrobromide and sodium benzoate and at 270 nm for paracetamole. The method was validated statistically for selectivity, linearity, precision, accuracy.
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