고체상 정제 및 HPLC/PDA에 의한 영유아식 중 나이아신의 분석

Abstract

This study was performed to establish a rapid and simple analytical method for niacin (nicotinic acid and nicotinamide) using HPLC. A pretreatment method for the extraction and clean-up of niacin in infant formula sample and an instrumental condition for HPLC were optimized. Niacin was extracted by 5 mM hexanesulfonate with ultrasonication for 30 min. For the clean-up of the sample, the extract was applied to a HLB cartridge, and then niacin was eluted from the cartridge using 5 mL of 80% methanol after washing with 5 mL of n-hexane. The total recoveries were 83～104% and relative standard deviation were in the range of 1.5～3.5% during the extraction and clean-up process. Niacin was determined by gradient elution with sodium hexanesulfonate/methanol buffer as a mobile phase and a photodiode array detector (260 nm). It showed a high linearity between the content of niacin and the peak area (r 2 =1.000) in the range of 0.02～10.0 mg/L of nicotinic acid and nicotinamide. The detection limit was 0.02 mg/L (0.2 mg/kg in the sample). The method was successfully applied for the determination of niacin in infant formula. Total niacin contents were in the range of 53.5～140.3 mg/kg.