快速溶剂萃取-在线固相萃取/高效液相色谱串联质谱法对复杂基体中壬基酚的测定

摘要

Samples of sediment,sludge and plants were extracted by ASE with a mixed solvent of dichloromethane,hexane and methanol (8∶1∶1,v/v/v).The extracts were on-line purified and enriched by SPE using Spark cartridges with methanol/water for elution,and then separated on an Agilent Poroshell 120 EC-C18 column using methanol and water (containing 0.1 ％ ammonia) as mobile phase for gradient elution.An Agilent 6420 triple quadrupole mass spectrometer was used for detection of NP on the negative ion multiple reactions monitoring (MRM) mode.The method showed desirable linearity in the concentration range of 0.25-75 ng,with correlation coefficients (r) no less than 0.999.The limit of detection (LOD) of the method was 0.05 ng.The method also exhibited favorable precision,with recoveries of 67.8％-82.6％ for soils samples and 65.9％-96.5％ for plants samples.10％ of the total samples were selected to be measured in parallel,and the relative deviation was within 0.1 ％-24.1％.The proposed method is simple,sensitive,automated,and suitable for rapid determination of trace NP in complex samples.%建立了测定复杂基体中壬基酚(Nonylphenol,NP)的快速溶剂萃取-在线固相萃取/高效液相色谱串联质谱分析方法.污泥、土壤及植物样品经冷冻干燥后,用正己烷、二氯甲烷、甲醇的混合溶剂(8∶1∶1,v/v/v)进行快速溶剂萃取;萃取液采用Spark在线固相萃取装置和配套在线固相萃取小柱进行在线富集和净化,以甲醇-0.1％氨水为流动相进行梯度洗脱,采用Agilent Poroshell 120 EC-C18高效液相色谱柱进行分离和分析.使用安捷伦6420三重四极杆串联质谱仪为质谱检测器,采用电喷雾电离源,以多反应监测(MRM)方式进行负离子模式监测,对复杂基体中NP进行定量分析.该方法NP线性范围为0.25～75 ng,相关系数r＞0.999,检出限为0.05 ng;该方法污泥样品的回收率为67.8％～82.6％,植物样的回收率为65.9％～96.5％;随机选取样品总数的十分之一进行平行样测定,相对偏差为0.1％～24.1％.该方法操作简单、灵敏,自动化程度高,可用于复杂基体中NP的快速测定.