邻-（2,3,4,5,6-五氟苄基）羟胺盐酸盐衍生-HPLC法测定果蔬中甲醛含量
Determination of formaldehyde in fruits and vegetables by HPLC derived with o-(2,3,4,5,6- pentafluorobenzyl) hydroxylamine hydrochloride
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摘要: 通过邻-（2,3,4,5,6-五氟苄基）羟胺盐酸盐与甲醛衍生,建立了测定果蔬中甲醛含量的高效液相色谱法。样品在温度为70℃超声波条件下直接提取衍生30 min,经离心纯化后液相色谱检测,外标法定量。优化的色谱条件为:Eelipse XDB-C18柱（4.6 mm×250 mm,5μm）;流动相为乙腈和水（70∶30,v/v）,流速1.0 m L/min,柱温40℃,检测波长210 nm。结果表明,该方法的检出限可达到0.114 mg/kg,在0.5757 mg/kg范围内呈良好的线性关系,平均回收率为82.3%94.1%,相对标准偏差为4.0%7.1%（n=6）。该方法样品前处理简便,稳定性好,检测限低,适合果蔬中甲醛的快速定量检测。Abstract: A high performance liquid chromatography method was used to determine formaldehyde in fruits and vegetables by o-( 2,3,4,5,6-pentafluorobenzyl) hydroxylamine hydrochloride derived with formaldehyde,Samples was directly extracted and derived at a temperature of 70 ℃ under the conditions of ultrasonic 30 min,then monitored by liquid chromatography after centrifugation and purified and quantified using the external standard method.The detection was performed on a XDB-C18 column( 4.6 mm × 250 mm,5 μm) in an isocratic elution mode using a mobile phase consisting of acetonitrile and water( 70∶ 30,v/v) at a flow rate of 1.0 m L/min,the column temperature was 40 ℃ and detection wavelength was 210 nm. The results showed that the quantification limit of the method was 0.114 mg/kg,with a good linear relationship between 0.57~57 mg/kg.The average recovery rate were 82.3% ~94.1%,with RSD of 4.0% ~8.1%( n = 6).The method was simple,stability,low detection limits and suitable for the determination formaldehyde in fruits and vegetables.
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