【摘要】 目的建立一种水中杀虫剂鱼藤酮的快速筛查方法,即利用超高效液相色谱-质谱(UPLC-MS)检测水样中鱼藤酮的方法。方法收集受污染的水样,用三氯甲烷振荡提取10 min,静置分层,取1 ml下层提取液经氮吹浓缩至近干后用1 ml乙腈溶解,溶解液过0.25μm滤膜后利用超高效液相色谱-质谱仪分离定性,外标法定量。结果在浓度为0.05μg/L～0.50μg/L时线性关系良好,线性方程为y=288 692x+641.932,线性相关系数(r)为0.999 2,方法的检出限以3倍标准差计算为0.60 ng/L,定量限以10倍标准差为2.0 ng/L。在低、中、高3种加标浓度水平下的回收率为63.8%～82.2%,相对标准偏差为3.01%～5.04%。结论本方法前处理操作简单快速,定性准确,检出限低,回收率高,精密度和准确度高。实际样品检测结果显示,本方法可以满足水样中鱼藤酮的快速筛查的要求。更多还原

【Abstract】 Objective To establish a method for the determination of pesticides rotenone in water samples by ultra high performance liquid chromatography-mass spectrometry(UPLC-MS). Methods The contaminated water was collected, and extracted by trichloromethane for 10 min, then stayed for layering, the lower chloroform extract was taken to pass a 0.25 um filtration membrane for qualification by UPLC-MS, and external standard method was adopted for quantification. Results Good linearity was obtained within 0.05 μg/L-0.50 μg/L, with linear equation y=288 692x+641.932 and with correlation coefficient(r) of 0.999 2. The minimum detectable concentration was 0.60 ng/L based on 3 times of the SD, The quantitative limit was 2.0 ng/L based on 10 times of the SD. The recoveries at the three levels of low, medium and high spiked concentrations were within 63.8%-82.2%, and the relative standard deviations were within 3.01%-5.04%. Conclusion The method is simple, accurate and high sensitive. The actual sample testing results showed that this method can meet the requirements in rapid screening pesticides rotenone.更多还原