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加速溶剂萃取-高效液相色谱法测定含脂羊毛中除虫脲和杀铃脲残留量

[Determination of diflubenzuron and triflumuron residues in greasy wool by accelerated solvent extraction technique and high performance liquid chromatography].

作者信息

Fan Yuanmu, Huang Shaotang, Yu Xuejun, Gu Xiaojun, Qiu Yajun, Chen Shubing, Fang Keteng, Chen Jun

机构信息

Ningbo Entry-Exit Inspection and Quarantine Bureau, Ningbo, China.

出版信息

Se Pu. 2009 Jul;27(4):463-6.

PMID:19938504
Abstract

A method for the determination of diflubenzuron and triflumuron residues in greasy wool was developed by high performance liquid chromatography (HPLC) coupled with accelerated solvent extraction (ASE). The diflubenzuron and triflumuron residues were extracted with acetonitrile saturated with n-hexane at 80 degrees C and 10.34 MPa. The extract was pretreated by a series of procedures such as freezing-lipid filtration, concentration and purification by solid-phase extraction prior to the determination with HPLC. The target analytes were separated on a Waters Atlants dC18 column (250 mm x 4.6 mm, 5 microm), gradiently eluted with acetonitrile and water as the mobile phases and detected by a photodiode array detector (DAD) at 254 nm. The linear ranges were 0.1 - 10.0 mg/L. There were good linearity between the peak areas and concentrations in the linear range for the analytes, and the correlation coefficients of diflubenzuron and triflumuron were higher than 0.9999. The limits of quantification for diflubenzuron and triflumuron were 0.05 and 0.04 mg/kg (S/N > or = 10), respectively. The method is simple, rapid, sensitive and suitable for preliminary screening of diflubenzuron and triflumuron residues in greasy wool.

摘要

建立了一种采用高效液相色谱(HPLC)结合加速溶剂萃取(ASE)测定含脂羊毛中除虫脲和杀铃脲残留量的方法。除虫脲和杀铃脲残留量在80℃和10.34MPa条件下用正己烷饱和的乙腈进行萃取。萃取液在采用HPLC测定之前,需经过冷冻除脂过滤、浓缩以及固相萃取净化等一系列预处理程序。目标分析物在Waters Atlants dC18柱(250mm×4.6mm,5μm)上进行分离,以乙腈和水作为流动相进行梯度洗脱,并采用光电二极管阵列检测器(DAD)在254nm波长处进行检测。线性范围为0.1 - 10.0mg/L。分析物在线性范围内峰面积与浓度之间具有良好的线性关系,除虫脲和杀铃脲的相关系数均高于0.9999。除虫脲和杀铃脲的定量限分别为0.05和0.04mg/kg(S/N≥10)。该方法简便、快速、灵敏,适用于含脂羊毛中除虫脲和杀铃脲残留量的初步筛查。

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