【摘要】 建立了温控离子液体分散液液萃取-液相色谱-串联质谱法(LC-MS/MS)测定环境水样中氯硝柳胺含量的分析方法。水样经离子液体萃取,以乙腈作为分散剂,通过温度控制加快离子液体分散液液萃取,经超声、离心、富集后,采用C18色谱柱进行分离,以乙腈-0.1%氨水溶液为流动相,梯度洗脱;质谱采用电喷雾负离子电离,多反应监测模式检测,定性离子对m/z324.9/171.1,定量离子对m/z324.9/289.0,外标法定量。结果表明:氯硝柳胺在5.0～200.0ng/mL浓度范围内与响应值线性关系良好,相关系数R~2为0.9998;当称样量为5.0mL时,检出限为0.15μg/kg,定量限为0.5μg/kg;回收率为91.7%～97.1%,相对标准偏差为0.8%～3.1%。该方法操作简单、精密度好、回收率高,可实现快速、批量和准确检测环境水体中氯硝柳胺含量。更多还原

【Abstract】 A method for the determination of niclosamide in environmental water samples by temperature controlled ionic liquid-dispersive liquid-liquid chromatography-liquid chromatography-tandem mass spectrometry(LC-MS)was established.Water samples were extracted by ionic liquid,and acetonitrile were used as dispersing agent.After being sonicated,centrifuged,and enriched,the residues were separated by C18 column,and acetonitrile and 0.1% aqueous ammonia solution was used as the mobile phase by gradient elution.Niclosamide were ionized by negative ion electrospray and detected by multireaction monitoring mode,and mass-to-charge ratios of qualitative ion pair and quantitative ion pair were m/z324.9/171.1 and m/z324.9/289.0,respectively.The results showed that the linear relationship were good in a concentration range of 5.0-200.0 ng/mL and correlation coefficient R~2 were 0.9998.When the sample amount was 5.0 mL,the detection limit was 0.15μg/kg,and the quantitative limit was 0.5μg/kg;the recovery were ranged from 91.7%to 97.1%,and the relative standard deviation(RSD)were ranged from0.8%to 3.1%.This method has the virtues of simple operation,good precision and high recovery,and it can realize rapid,batch and accurate determination of niclosamide in environmental water.更多还原