Shim You-Shin, Kim Seunghee, Seo Dongwon, Ito Masahito, Nakagawa Hiroaki, Park Hyun-Jin, Ha Jaeho
Korea Food Research Institute, Food Analysis Center, 516, Baekhyeon, Bundang, Seongnam, Gyeonggi, 463-746, Republic of Korea.
J AOAC Int. 2013 Sep-Oct;96(5):1059-64. doi: 10.5740/jaoacint.12-439.
A rapid method for the simultaneous determination of flavonol aglycones in food using ultra-high-performance LC (u-HPLC) coupled with a heating-block acidic hydrolysis method was validated in terms of precision, accuracy, and linearity. The u-HPLC separation was performed on an RP C18 column (particle size 2 micro m id, 2 mm, length 100 mm) with a photodiode array detector. The LOD and LOQ of the u-HPLC analyses were 0.15 and 0.47 mg/kg for myricetin, 0.09 and 0.28 mg/kg for quercetin, 0.16 and 0.49 mg/kg for kaempferol, and 0.08 and 0.25 mg/kg for isorhamnetin. The intraday and interday precisions of the individual flavonol aglycones were less than 9.31%. All calibration curves exhibited good linearity (r2 = 0.99) within the tested ranges. Total run time of u-HPLC was 13 min. The rapid u-HPLC method presented herein significantly improved the speed, sensitivity, and resolution of the analyses of myricetin, quercetin, kaempferol, and isorhamnetin in food.
采用超高效液相色谱(u-HPLC)结合加热块酸性水解法同时测定食品中黄酮醇苷元的快速方法,在精密度、准确度和线性方面得到了验证。u-HPLC分离在配有光电二极管阵列检测器的RP C18柱(粒径2μm,内径2mm,长度100mm)上进行。u-HPLC分析中杨梅素的检测限和定量限分别为0.15和0.47mg/kg,槲皮素为0.09和0.28mg/kg,山奈酚为0.16和0.49mg/kg,异鼠李素为0.08和0.25mg/kg。各黄酮醇苷元的日内和日间精密度均小于9.31%。所有校准曲线在测试范围内均表现出良好的线性(r2 = 0.99)。u-HPLC的总运行时间为13分钟。本文提出的快速u-HPLC方法显著提高了食品中杨梅素、槲皮素、山奈酚和异鼠李素分析的速度、灵敏度和分辨率。