Journal of the Korean Society of Food Science and Nutrition (한국식품영양과학회지)

The Korean Society of Food Science and Nutrition (한국식품영양과학회)
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Determination of Niacin in Infant Formula by Solid-phase Clean-up and HPLC with Photodiode Array Detector

고체상 정제 및 HPLC/PDA에 의한 영유아식 중 나이아신의 분석

  • Hong, Jee-Eun (Center for Food and Drug Analysis, Gyeongin Regional Food & Drug Adminstration) ;
  • Kim, Mi-Ran (Center for Food and Drug Analysis, Gyeongin Regional Food & Drug Adminstration) ;
  • Cheon, Sang-Hee (Center for Food and Drug Analysis, Gyeongin Regional Food & Drug Adminstration) ;
  • Chai, Jung-Young (Center for Food and Drug Analysis, Gyeongin Regional Food & Drug Adminstration) ;
  • Park, Eun-Ryong (Center for Food and Drug Analysis, Gyeongin Regional Food & Drug Adminstration) ;
  • Mun, Chun-Sun (Center for Food and Drug Analysis, Gyeongin Regional Food & Drug Adminstration) ;
  • Gwak, In-Shin (Food Safety Evaluation Department, Korea Regional Food & Drug Adminstration) ;
  • Kim, Ok-Hee (Center for Food and Drug Analysis, Gyeongin Regional Food & Drug Adminstration) ;
  • Lee, Kwang-Ho (Food Safety Evaluation Department, Korea Regional Food & Drug Adminstration)
  • 홍지은 (경인지방식품의약품안전청 시험분석센터) ;
  • 김미란 (경인지방식품의약품안전청 시험분석센터) ;
  • 천상희 (경인지방식품의약품안전청 시험분석센터) ;
  • 채정영 (경인지방식품의약품안전청 시험분석센터) ;
  • 박은령 (경인지방식품의약품안전청 시험분석센터) ;
  • 문춘선 (경인지방식품의약품안전청 시험분석센터) ;
  • 곽인신 (식품의약품안전청 식품평가부) ;
  • 김옥희 (경인지방식품의약품안전청 시험분석센터) ;
  • 이광호 (식품의약품안전청 식품평가부)
  • Published : 2009.03.31
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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 $83{\sim}104%$ and relative standard deviation were in the range of $1.5{\sim}3.5%$ 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 $0.02{\sim}10.0$ 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 $53.5{\sim}140.3$ mg/kg.

영유아식 중 나이아신의 기기분석법을 개발하고 영 유아식 중의 나이아신의 함량을 조사하였다. 니코틴산 및 니코틴 아미드에 대해 액체 추출 및 고체상 정제과정을 통해 전처리 한 후 HPLC로 분석할 경우 $83{\sim}104%$ 범위의 회수율과 $1.5{\sim}3.5%$ 범위의 재현성을 나타내었다. 또한 260 nm의 파장에서 분석할 경우 $0.02{\sim}10$ mg/L 범위에서 검량선의 직선성이 1.0000 수준으로 매우 높게 나타났으며 영유아식 중의 검출 한계는 0.2 mg/kg 수준으로 나타났다. 총 50건의 영 유아식에 대해 나이아신 함량을 모니터링한 결과 $53.5{\sim}140.3$ mg/kg 수준으로 나타났으며 3회 반복시험 시의 상대표준편차는 $0.6{\sim}5.5%$ 범위로 나타나 본 방법이 나이아신 분석에 유용한 방법임을 확인하였다.

Keywords

References

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