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

作　　者：奉夏平[1] 曾宪远[1] 付丽敏[1] 唐丽娜[1] 黄秀丽[1] 陈清清[1] 

机构地区：[1]广东省惠州市质量计量监督检测所,广东惠州516003

出　　处：《现代食品科技》2013年第8期2025-2029,共5页Modern Food Science and Technology

基　　金：广东省惠州市科技局资助项目(2011g031)

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1.2-4.0μg/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0.5mg/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。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 Cl8 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 ~tg/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.

关 键 词：高效液相色谱法 柑橘 防腐保鲜剂 残留量 

分 类 号：TS255.7[轻工技术与工程—农产品加工及贮藏工程] O657.72[轻工技术与工程—食品科学与工程]