摘要
采用分散固相萃取（QuEChERS）为样品前处理方法,建立了高效液相色谱-串联质谱（HPLC-MS/MS）快速检测烟叶和土壤中新型杀菌剂壬菌铜残留的分析方法。考察了破络剂对壬菌铜的破络效果以及不同分散固相吸附剂对净化效果的影响。样品中的壬菌铜经硫化钠破络、乙腈提取、N-丙基乙二胺吸附剂（PSA）净化后,以乙腈-水作为流动相进行梯度洗脱,电喷雾正离子（ESI＋）模式电离,三重四极杆串联质谱以多反应监测模式（MRM）进行测定。结果表明,在0.001-1.0 mg·L^-1浓度范围内线性关系良好,不同基质中壬菌铜解络产物——壬基酚磺酸的线性系数均大于0.99。在0.01-2.0 mg·kg^-1加标水平下,壬菌铜在鲜烟叶、干烟叶和土壤中的平均回收率分别为84.7%-92.5%,87.1%-103.2%,83.0%-90.9%,相对标准偏差（RSD）分别为6.9%-8.3%,5.8%-10.6%,6.0%-9.0%。仪器的检出限为5.5×10^-5mg·kg^-1,方法的定量下限为0.01 mg·kg^-1。该方法简便、快速、准确,可用于烟叶和土壤中壬菌铜残留量的检测。
A rapid and sensitive analytical method for the determination of cuppric nonyl phenolsulfonate residues in tobacco and soil samples was developed and validated based on QuEChERS（Quick,Easy,Cheap,Effective,Rugged and Safe） and high performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS）.Factors affecting the decomplexation efficiency by different compounds were investigated.The effects of type and volume of dispersive solvent on the clean up of tobacco and soil extracts were also assessed.Residues in the samples were decomplexated by sodium sulfide,extracted with acetonitrile and then cleaned up with primary secondary amine（PSA）.The product nonyl phenol sulfonic acid in the extract was separated by gradient elution using a mobile phase of acetonitrile-water and then analyzed by electrospray ionization in positive ion mode（ESI＋） under multiple reaction monitoring（MRM） mode.Linearity was assessed by calibration curve in blank matrix to compensate for matrix effect.Good linearities（r 〉0.99） were obtained for nonyl phenol sulfonic acid in the matrix matched standards in the range of 0.001-1.0 mg·L^-1.The average recoveries at spiked levels of 0.01-2.0 mg·kg^-1 were in the range of 84.7%-92.5% for green tobacco leaf,87.1%-103.2% for dried tobacco leaf and 83.0%-90.9% for soil,with relative standard deviations（RSDs） of 6.9%-8.3%,5.8%-10.6% and 6.0%-9.0%,respectively.The limits of detection（LOD） were 5.5×10^-5 mg·kg^-1,while the limits of quantitation（LOQ） were determined as 0.01 mg·kg^-1 for green,dried tobacco leaf and soil.This method is easy,quick and effective,and could be applied in the determination of cupric nonyl phenolsulfonate in tobacco and soil samples.
出处
《分析测试学报》
CAS
CSCD
北大核心
2015年第1期91-95,共5页
Journal of Instrumental Analysis
基金
国家自然科学基金项目(41201291)
中央级公益性科研院所基本科研业务费专项(2012ZL056)
国家烟草专卖局重点项目(TS-06-20110039
110200902073)
关键词
QUECHERS
高效液相色谱-串联质谱
壬菌铜
烟叶
土壤
QuEChERS
high performance liquid chromatography- tandem mass spectrometry（ HPLC - MS/MS）
cuppric nonyl phenolsulfonate
tobacco
soil
