高效液相色谱法测定柑橘中6种防腐保鲜剂的残留

Detection of 6 Preservative Residues of in Orange by High Performance Liquid Chromatography

摘要:

建立了同时对柑橘中6种防腐保鲜剂包括对羟基苯甲酸甲酯（尼泊金甲酯）、对羟基苯甲酸乙酯（尼泊金乙酯）、乙萘酚、4-苯基苯酚、2,4-二氯苯氧乙酸（2,4-D）和联苯醚（二苯醚）残留量进行测定的高效液相色谱法。样品经乙醚提取后，活性炭柱净化。C18 色谱柱分离，流动相为甲醇:水（55:45，磷酸调节pH≈3），二极管阵列检测器，检测波长为208 nm。结果表明：6种标准物质在1.2~4.0 μg/mL范围内呈良好线性关系，相关系数均可达到0.999，在此范围内，各防腐保鲜剂的加标回收率在85.65~106.50%之间，相对标准偏差为2.36%~6.78%。该方法中乙萘酚的检测限为0.5 mg/kg，对羟基苯甲酸甲酯、对羟基苯甲酸乙酯、2,4-D、4-苯基苯酚和联苯醚的检测限为1.0 mg/kg。该方法简便，快速、准确、灵敏度高、重现性好，能满足柑橘中6种防腐保鲜剂残留量的检测要求。

Abstract:

A method was established to detect 6 kinds of fruit preservatives including p-methyl hydroxybenzoate, p-ethyl hydroxybenzoate, ethyl naphthol ,4-phenyl phenol,2,4-dichlorobenzene oxygen ethanoic acid (2,4-D) and diphenyl ether in orange by High Performance Liquid Chromatography (HPLC). The samples were extracted by ether and purified by activated carbon column and analyzed on a reversed phase C18 column using 55% CH3OH-45% H2O (pH 3) as mobile phase with a Diode array detector at 208 nm. The calibration curves showed good linear relatioship between the peak areas and concentrations of 6 preservatives in the range of 1.2~4.0 μg/mL, with correlation coefficients more than 0.999. Standard addition recovery ranged from 85.65% to 106.50% with relative standard deviation (RSD) from 2.36% to 6.78%. The limit of detection of ethyl naphthol was 0.5 μg/kg and the other five were 1.0 μg/kg. The method was simple, rapid and accurate, with high sensitivity and reproducibility, which was suitable for the analysis of the 6 preservatives mentioned above in orange.