摘要
建立了一种测定6类液体农药制剂中烷基酚(alkylphenols,APs)及其聚氧乙烯醚类(alkylphenol ethoxylates,APEOs)助剂的高效液相色谱-荧光分析方法。乳油、水剂、水乳剂、悬浮剂、可溶液剂和微乳剂样品均经甲醇超声辅助提取,稀释后过聚丙烯膜,采用Poroshell 120EC-C_(18)(4.6 mm×100 mm,2.7μm)分离,V(甲醇):V(乙腈):V(水)=75.5:6.5:18.0三元流动相等度洗脱,荧光检测器检测,外标法定量。结果表明:在0.05~10或0.1~20mg/L范围内,APs和APEOs的峰面积与其质量浓度间呈良好线性关系(R^2均大于0.999 8);在添加水平范围内(APs:0.5、2、5 mg/g;APEOs:1、5、25、50mg/g),6类液体农药剂型中APs和APEOs的平均回收率为73%~110%,相对标准偏差为0.6%~14.9%,方法的定量限在0.5~1mg/g。该方法简单、快速、准确,适用于不同液体农药制剂中烷基酚及其聚氧乙烯醚类助剂的测定。
A simple method for simultaneous determination of alkylphenols （APs） and alkylphenol ethoxylates （APEOs） in six kinds of liquid pesticide formulations was developed using high- performance liquid chromatography with fluorescence detection （HPLC-FLD）. Six kinds of liquid pesticide formulation samples （emulsifiable concentrate, aqueous solutions, emulsion in water, suspension concentrate, soluble concentrate, and microemulsion） were ultrasonically extracted with methanol. The extract was diluted with methanol and centrifuged. The supematant was filtered through a polypropylene （PP） filter and then separated on an Agilent Poroshell C18 （4.6 mm × 100 mm, 2.7 μm） chromatographic column using an isocratic elution program of V （methanol）： V （acetonitrile）： V （water） =75.5 ： 6.5 ： 18.0. Qualitative analysis was performed by HPLC-FLD, and the external standard method was used to quantify the concentrations of target analytes. The results showed that good linearity between the peak areas of APs and APEOs and their mass concentrations （R2〉0.999 8） was obtained in the range of 0.05-10 and 0.1-20 mg/L. At three or four spiked levels （APs： 0.5, 2, 5 mg/g; APEOs： 1, 5, 25, 50 rag/g）, the mean recoveries ranged from 73% to 110%, with relative standard deviations （RSD, n = 5） of 0.6%-14.9% in those six kinds of liquid pesticide formulations. The limits of quantitation （LOQ） varied from 0.5 mg/g to 1 mg/g. This new method is convenient, rapid, accurate and suitable for the simultaneous determination of APs and APEOs in those six kinds of liquid pesticide formulations.
作者
江泽军
曹晓林
李辉
张婵
金芬
佘永新
王静
JIANG Zejun CAO Xiaolin LI Hui ZHANG Chan JIN Fen SHE Yongxin WANG Jing(Institute of Quality Standard and Testing Technology for Agro-products, Chinese Academy of Agricultural Sciences,＂ Key Laboratory of Agro-product Quality and Safety, Ministry of Agriculture, Beijing 100081, China)
出处
《农药学学报》
CAS
CSCD
北大核心
2017年第2期245-253,共9页
Chinese Journal of Pesticide Science
基金
科技部科技基础性工作专项项目(2013FY110100)
中国农业科学院科技创新工程"农业化学污染物残留检测及行为研究"创新团队
关键词
农药助剂
液体农药制剂
烷基酚
烷基酚聚氧乙烯醚
高效液相色谱
pesticide adjuvants
liqvuid pesilicide formulations
alkylphenols （APs）
alkylphenolethoxylates （APEOs）
high-performance liquid chromatography （HPLC）
