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오미현,임무성,채정영,김은정,조중훈,임철수,최선옥 한국식품위생안전성학회 2017 한국식품위생안전성학회지 Vol.32 No.2
A rapid, sensitive analytical method for glucuronolactone in beverages was developed and validated using hydrophilic interaction liquid chromatography coupled to electrospray ionization tandem mass spectrometry (HILIC-ESI-MS/MS). To determine the optimum analytical conditions for glucuronolactone, three different kinds of HILIC columns and two mobile phases with different pH values were examined. An amide-bonded stationary phase with a pH 9 acetonitrile-rich mobile phase was the best condition in terms of column retention, ESI-MS/MS response area, and signal-to-noise ratio. After extraction, glucuronolactone was separated through the HILIC amide column and detected by negative ESI-MS/MS in selected reaction monitoring (SRM) mode. Nine energy drinks sold in Korea were spiked with glucuronolactone at a concentration of 5 ng/mL; the Monster EnergyTM sample showed the smallest peak area and its signal-to-noise ratio was used for method validation. Good linearity was obtained in the concentration range from 20 to 1500 ng/mL with a correlation coefficient > 0.998. The developed method had a limit of detection (LOD) of 6 ng/mL and a limit of quantitation (LOQ) of 20 ng/mL. The recovery of this method at concentration of 20, 100, 500, and 1000 ng/mL was 96.3%-99.2% with relative standard deviations (RSD) of 1.6%- 14.0%. A reproducibility precision assessment at concentration of 100 and 500 ng/mL was carried out among three laboratories. The recovery of that evaluation was 95.1%-102.3% with RSD of 2.7%-7.0%. An analysis of variance indicated that there was no difference between the recovery results of the three laboratories at the 5% significance level. The validated method is applicable to inspecting beverages adulterated with glucuronolactone in Korea.
고체상 정제 및 HPLC/PDA에 의한 영유아식 중 나이아신의 분석
홍지은(Jee Eun Hong),김미란(Miran Kim),천상희(Sanghee Cheon),채정영(Jungyoung Chai),박은령(Eun Ryong Park),문춘선(Chun Sun Mun),곽인신(In-Shin Gwak),김옥희(Ok-Hee Kim),이광호(Kwang Ho Lee) 한국식품영양과학회 2009 한국식품영양과학회지 Vol.38 No.3
영유아식 중 나이아신의 기기분석법을 개발하고 영ㆍ유아식 중의 나이아신의 함량을 조사하였다. 니코틴산 및 니코틴아미드에 대해 액체 추출 및 고체상 정제과정을 통해 전처리한 후 HPLC로 분석할 경우 83~104% 범위의 회수율과 1.5~3.5% 범위의 재현성을 나타내었다. 또한 260 ㎚의 파장에서 분석할 경우 0.02~10 ㎎/L 범위에서 검량선의 직선성이 1.0000 수준으로 매우 높게 나타났으며 영유아식 중의 검출한계는 0.2 ㎎/㎏ 수준으로 나타났다. 총 50건의 영ㆍ유아식에 대해 나이아신 함량을 모니터링한 결과 53.5~140.3 ㎎/㎏ 수준으로 나타났으며 3회 반복시험 시의 상대표준편차는 0.6~5.5% 범위로 나타나 본 방법이 나이아신 분석에 유용한 방법임을 확인하였다. 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 ㎚). It showed a high linearity between the content of niacin and the peak area (r²=1.000) in the range of 0.02~10.0 ㎎/L of nicotinic acid and nicotinamide. The detection limit was 0.02 ㎎/L (0.2 ㎎/㎏ 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 ㎎/㎏.