摘要
建立了荔枝中对氯苯氧乙酸(钠)残留量的液相色谱和液相-串联质谱检测方法,采用碱性水提取,利用二氯甲烷液液萃取进行净化,用液相色谱方法在280 nm检测,检出限为0.02 mg/kg。在负离子模式下进行液质串联质谱检测,检出限为0.01 mg/kg。本方法的添加回收率在78.2%~106.7%,变异系数为2.0%~12.2%。回收率、检测限等技术参数均能满足相关检测要求。本方法应用于65个实验样品的检测,其中有两个样品为阳性,含量分别为0.032 mg/kg及0.026 mg/kg。
A sensitive and selective analytical method for the determination of(sodium) parachlorophenoxy acetate(sodium 4-CPA) in lichee by high-performance liquid chromatography(HPLC) and liquid chromatography/tandem mass spectrometry(LC-MS/MS) was developed.The sample was extracted with water(pH 10) and the extract was cleaned up with dichloromethane.The LOQs were 0.02 and 0.01 mg/kg for HPLC and LC-MS/MS,respectively.The RSDs of recovery for indoxacarb were 2.0 %-12.2 % in lichee.Six repetitive determinations of recovery achieved good reproducibility for sodium 4-CPA and the recovery ranged from 78.2 %-106.7 %.The proposed procedure was applied to the analysis of several real samples of different origin from Fujian Province,and 65 samples were screened for indoxacarb residue,of which 2 positive samples were found.
出处
《检验检疫科学》
2010年第2期24-27,共4页
Inspection and Quarantine Science
基金
福建省自然基金青年创新项目(2006F3002)
国家质检总局科技项目(2007IK146)
厦门市科技计划项目(3502Z20072003
3502Z20092008
3502Z20092009)
关键词
对氯苯氧乙酸钠
液相色谱法
液相-串联质谱法
(Sodium) parachlorophenoxy Acetate
High-Performance Liquid Chromatography(HPLC)
Liquid Chromatography/Tandem Mass Spectrometry(LC-MS/MS)