快速溶剂萃取-高效液相色谱法测定含脂羊毛中残留的除虫脲和杀铃脲

色谱 , 2009, 27(4): 463-466. doi: 10.3321/j.issn:1000-8713.2009.04.016

快速溶剂萃取-高效液相色谱法测定含脂羊毛中残留的除虫脲和杀铃脲

樊苑牧 ^1, , 黄绍棠 ^2, , 俞雪钧 ^3, , 顾晓俊 ^4, , 裘亚钧 ^5, , 陈树兵 ^6, , 房科腾 ^7, , 陈俊 ^8,

1.宁波出入境检验检疫局,浙江,宁波,315012

2.宁波出入境检验检疫局,浙江,宁波,315012

3.宁波出入境检验检疫局,浙江,宁波,315012

4.宁波出入境检验检疫局,浙江,宁波,315012

5.宁波出入境检验检疫局,浙江,宁波,315012

6.宁波出入境检验检疫局,浙江,宁波,315012

7.宁波出入境检验检疫局,浙江,宁波,315012

8.宁波出入境检验检疫局,浙江,宁波,315012

基金项目: 国家质量监督检验检疫总局科研项目(2006IK021)

关键词：快速溶剂萃取 , 高效液相色谱法 , 除虫脲 , 杀铃脲 , 含脂羊毛 , 杀虫剂

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

建立了快速溶剂萃取-高效液相色谱(ASE-HPLC)测定含脂羊毛中除虫脲、杀铃脲残留量的方法.以正己烷饱和的乙腈为萃取剂,在80 ℃、10.34 MPa条件下用快速溶剂萃取仪提取样品中的目标物,提取液经冷冻除脂、浓缩及Waters Plus Silica柱净化后,采用Waters Atlants dC18色谱柱分离,以乙腈和水为流动相进行梯度洗脱,二极管阵列检测器于254 nm处检测.结果表明,在0.1～10.0 mg/L 范围内,除虫脲、杀铃脲的峰面积与其质量浓度的线性关系良好,相关系数均大于 0.999 9,定量检出限(S/N≥10)分别为0.05,0.04 mg/kg.该方法具有操作简便、快速、灵敏度高等特点,完全能满足含脂羊毛中除虫脲、杀铃脲残留初筛检测的要求.

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