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作 者:奉夏平[1] 宁焕焱[1] 黄飞[1] 付丽敏[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:《分析测试学报》2013年第12期1482-1486,共5页Journal of Instrumental Analysis
基 金:广东省惠州市科技局资助项目(2011g031)
摘 要:建立了高效液相色谱-串联质谱法同时测定对羟基苯甲酸甲酯、对羟基苯甲酸乙酯、2,4-二氯苯氧乙酸(2,4-D),乙萘酚和4-苯基苯酚5种鲜水果保鲜剂残留量的分析方法。样品经乙醚提取,固相萃取活性炭柱净化后,C18色谱柱分离,以乙腈和50%甲醇水为流动相进行梯度洗脱,电喷雾负离子(ESI-)模式电离,液相色谱-质谱法(LC-MS/MS)测定。结果表明:5种保鲜剂在0.05~1.2 mg/L范围内呈现良好的线性关系,相关系数(r^2)均大于0.999,5种保鲜剂的检出限为0.5~20μg/kg。方法的加标回收率为81.0%~104.5%,相对标准偏差(RSD)为1.3%~6.8%。该方法简便快捷、灵敏度及准确性高,可满足鲜水果防腐保鲜剂残留量检测的要求。A high performance liquid chromatography coupled with tandem mass spectrometric( HPLC- MS / MS) method was established to detect residues of 5 fruit preservatives including p-methyl hydroxybenzoate,p-ethyl hydroxybenzoate,2,4-dichlorobenzene oxygen ethanoic acid( 2,4-D), ethyl naphthol and 4-phenyl phenol simultaneously. The samples were extracted with ether,then purified with activated carbon column,and separated on a C 18 column by gradient elution using 50% methanol( A)- acetonitrile( B) as mobile phase. The calibration curves were linear between peak areas and concentrations of 5 preservatives in the range of 0. 05-1. 2 mg / L,with correlation coeffi- cients more than 0. 999. The limits of detection were in the range of 0. 5- 2. 0 μg / kg for five preservatives. The average recoveries ranged from 81. 0% to 104. 5%,with RSDs of 1. 3%- 6. 8%. The method was suitable for the analysis of the above preservatives in fresh fruits with advantages of rapidness,good sensitivity and accuracy.
关 键 词:高效液相色谱-串联质谱 鲜水果 防腐保鲜剂 残留量
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