摘要
建立了高效液相色谱一质谱／质谱（HPLC-MS／MS）测定渔业水体中氯硝柳胺残留量的分析方法。水样加入0．2％乙酸酸化，用乙腈振荡提取，再用二氯甲烷液液萃取。提取液旋转蒸发仪浓缩，流动相复溶后，HPLC-MS／MS下采用负离子电喷雾离子源（ESI^-）在选择反应监测（RSM）检测，外标法定量。在0．5～100μg／L范围内，峰面积与质量浓度线性良好，线性相关系数为0．9996；检出限为0．1μg/L。样品加标回收率为95．0％～100．6％，相对标准偏差为1．9％～6．9％，符合药物残留量分析的技术要求。
A method was established for the analysis of niclosamide residue in water by high performance liquid chromatography tandem mass spectrometry （HPLC-MS/MS） . The water samples were acidified by 0. 2% acetic acid and extracted with acetonitrile, and then liquid-liquid extracted with dichloromethane. The samples were analyzed by HPLC-MS/MS in selective reaction monitoring （SRM） mode via negatively polarity electrospray ionization （ ESI - ）. The external standard method was used for the quantification. The linear range was from 0. 5 to 100 μg/L with a good linear relationship （ R^2 =0. 9996）. The limit of quantification （LOQ） was 0.1 μg/mL, and it is better than the other methods, so it is more suitable for the detection of trace level of niclosamide in basal complex biological materials. The recoveries of this method were from 95.0 to 100. 6% with the relative standard deviations of 1.9% -6. 9% , and can meet the requirement of the determination of pesticide residues.
出处
《分析试验室》
CAS
CSCD
北大核心
2015年第1期53-56,共4页
Chinese Journal of Analysis Laboratory
关键词
氯硝柳胺
高效液相色谱-质谱/质谱法
渔业水体
Niclosamide
High performance liquid chromatography-mass spectrometry/mass spectrometry
Fishery water.
