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超局效液相法测定果蔬中的甲酸

The Determination of Formaldehyde in Fruits and Vegetables by Ultra High-performance Liquid Chromatography
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摘要 通过研究甲醛与2 ,4-二硝基苯肼发生衍生反应,经超高效液相色谱分离,二极管阵列检测器和保留时间定性, 可对果蔬中的甲醛进行准确地定性定量测定.优化的色谱条件为ACQUITY UPLC CSH C18色谱柱( 2.1mm×100mm,1.7jum), 流动相甲醇- 水( 55:45 v/v), 流动相流速0 .25mL/min, 检测时间7.0min, 柱温40 ℃ , 检测波长354nm, 衍生提取反应 温度60℃.该方法的定量检测限为0.0089mg/kg,在0.005-1.000mg/L范围内呈现良好的线性关系.当甲醛添加量分别为 0.02、0.18、1.80mg/kg时,平均回收率为78.2%~94.8%,相对标准偏差为3.1%~6.5% (n = 6 ).该方法样品前处理简便、 稳定性良好、定量限低,能满足果蔬中甲酸含量的检测要求. A high performance liquid chromatography (HPLC) method was used to determine formaldehyde in fruits and vegetables by fomaldehyde derivation with 2,4-dinitrophenylhydrazine. The quantitation was perfomed by W method. The separation was performed on an ACQUITY UPLC CSH Cl8 column (2.1 mm×100 mm, 1.7 μm) in an isocratic elution mode using a mobile phase consisting of methanol and water (55:45, V/V) at a flow rate of 0.25 mL/min. The column temperature was 40 ℃ and detection wavelength was 354 nm. The best derivative extraction reaction temperature was 60 ℃ . The results showed that the limit of quantification (LOQ) of the presented method was 0.0089 mg/kg, with a good linear relationship in the range of 0.005? 1.000 mg/L. The average recovery rates at three spiked levels were 78.2%-94.8%,with relative standard derivation (RSD) of 3.1 %-6.5% (n = 6) at three spiking levels of 0.02、0.18、1.80mg/kg. The method was stable, simple and suitable for the determination of formaldehyde in fruits and vegetables with a low limit of detection (LOD).
作者 郑智恩 何如意 滕焕勇 张培培 ZHENG Zhi-en;HE Ru-yi;TENG Huan-yong;ZHANG Pei-pei(Wenzhou Vocational College of Science and Technology, WenZhou,Zhejiang 32500)
出处 《温州科技职业学院学报》 2017年第2期26-28,共3页 Journal of WenZhou Vocational College of Science And Technology
关键词 超高效液相 甲醛 果蔬 衍生反应 二极管阵列 UPLC formaldehyde fruits and vegetables formaldehyde derivative
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