高效液相色谱法测定果蔬中的5种农药残留 - 食品安全质量检测学报.docVIP

高效液相色谱法测定果蔬中的5种农药残留 仲伶俐, 李 曦, 李华仙, 付成平, 赵 珊, 雷欣宇 四川省农业科学院分析测试中心, 成都 610066 摘 要: 目的 建立高效液相色谱果蔬中啶虫脒、嘧霉胺、氟虫腈、辛硫磷和哒螨灵5种农药残留。方法 样品以乙腈为提取剂, NH2固相萃取小柱净化和富集, 用二氯甲烷-甲醇(97:3, V:V)溶液进行洗脱, 洗脱液浓缩、定容后, 以Dikma Spursil C18(250 mm×4.6 mm, 5 μm)色谱柱分离, 水和甲醇为流动相梯度洗脱, 流速为1.0 mL/min, 于配有紫外可变波长检测器的高效液相色谱仪测定, 外标法定量。结果5种农药在0.1~2.0 μg/mL的浓度范围内具有良好的线性关系, 相关系数为0.9995~0.9998。方法定量限为0.006~0.02 mg/kg。当添加浓度在0.02、0.05、0.1 mg/kg时, 5种农药在果蔬中的加标回收率达到70.2%~113.0%, 相对标准偏差为2.0%~11.8%。结论该方法操作简单、快速, 适用于果蔬中啶虫脒、嘧霉胺、氟虫腈、辛硫磷和哒螨灵残留的测定。 关键词高效液相色谱; 果蔬; 农药残留 Determination of 5 pesticide residues in fruits and vegetables by high performance liquid chromatography ZHONG Ling-Li*, LI Xi, LI Hua-Xian, FU Cheng-Ping, ZHAO Shan, LEI Xin-Yu (Analysis and Testing Center of Sichuan Academy of Agricultural Sciences, Chengdu 610066, China) ABSTRACT: Objective To establish a method for the determination of 5 kinds of pesticide residues (acetamiprid, pyrimethanil, fipronil, phoxim and pyridaben) in fruits and vegetables by high performance liquid chromatography (HPLC). Methods The samples were treated with acetonitrile as the extractant, then cleaned up and concentrated by NH2 solid phase extraction (SPE), and eluted with dichloromethane-methanol (97:3, V/V). The samples were separated by a Dikma Spursil C18 column (250 mm×4.6 mm, 5 μm) at the flow rate of 1.0 mL/min using water and methanol as mobile phase for the gradient elution. The target compounds were determined by HPLC equipped with an ultraviolet variable wavelength detector, and then quantitatively analyzed by external standard method. Results Five kinds of pesticides had good linear relationships between peak areas and concentrations in the concentration range of 0.1~2.0 μg/mL, and the correlation coefficients were 0.9995~0.9998. The limits of quantification (LOQs) were 0.006~0.02 mg/kg. The recoveries of 5 pesticides in fruits and vegetables reached 70.2%~113.0% when spiked at 0.02, 0.05 and 0.1 mg/kg, with relative standard deviations of 2.0%~11.8%. Conclus