Ivanova Bojidarka, Spiteller Michael
Lehrstuhl für Analytische Chemie, Institut für Umweltforschung, Fakultät für Chemie, Universität Dortmund, Otto-Hahn-Straße 6, 44227, Dortmund, Nordrhein-Westfalen, Germany,
Environ Geochem Health. 2015 Jun;37(3):557-74. doi: 10.1007/s10653-014-9673-9. Epub 2015 Jan 3.
The work presented here refers firstly to solid-state UV-MALDI-Orbitrap-mass spectrometric analysis of fluroxypyr (A) and triclopyr (B) in soils under laboratory conditions. The experimental design has involved the following: (a) determination of analytes A and B in polycrystalline composites of organic materials 1-7, based on 2-piperidine (pyrrolidine or piperazine)-1-yl-ethyl ammonium salts in order to determine the effect of sample preparation techniques on method performance using commercial herbicide formulations and (b) analysis of non-(X j,k,l (i) ) and sterilized (Y j,k,l (i) ) soil samples (i-fold rate 1, 10, 100, or 1,000; j-pesticide type A or B; k-time (0, 5, 10, 20, and 50 days) and l = 1-3 replicated samples) having clay content ∈ 5.0-12.0 %, silt ∈ 23.0-51.1 %, sand ∈ 7.2-72.0 %, and pH ∈ 4.0-8.1. In order to obtain a high representativeness of the data toward real-field experiments, the pollution scheme has involved 1-, 10-, 100-, and 1,000-fold rates. The firstfold rate has concentration of pollutant A of 2.639 × 10(-4) g in 625 cm(2) soil horizon of 0-25 cm(2) (5 cm depth) according to registration report (PSM-Zulassungbericht) of German Federal Office of Consumer Protection and Food Safety (Bundesamt für Verbraucherschutz und Lebensmittelsicherheit) 6337/26.10.2009. The experimental design has involved quincunx systematic statistical approach for collection of soil samples. The performance has been compared with the corresponding statistical variable obtained, using an independent HPLC-ESI-(APCI-)-MS/MS analysis.
本文介绍的工作首先涉及在实验室条件下对土壤中氟草烟（A）和绿草定（B）进行固态紫外基质辅助激光解吸电离傅里叶变换离子回旋共振质谱分析。实验设计包括以下内容：（a）基于2-哌啶（吡咯烷或哌嗪）-1-基-乙基铵盐，测定有机材料1-7多晶复合物中的分析物A和B，以使用商业除草剂配方确定样品制备技术对方法性能的影响；（b）分析非（X j,k,l (i) ）和灭菌（Y j,k,l (i) ）土壤样品（i倍率为1、10、100或1000；j为农药类型A或B；k为时间（0、5、10、20和50天），l = 1-3个重复样品），其粘土含量为5.0-12.0%，粉砂含量为23.0-51.1%，砂含量为7.2-72.0%，pH值为4.0-8.1。为了使数据对实际田间实验具有高度代表性，污染方案涉及1倍、10倍、100倍和1000倍率。根据德国联邦消费者保护和食品安全办公室（Bundesamt für Verbraucherschutz und Lebensmittelsicherheit）2009年10月26日的注册报告（PSM-Zulassungbericht）6337，在0-25平方厘米（5厘米深度）的625平方厘米土壤层中，第一倍率的污染物A浓度为2.639×10(-4)克。实验设计采用梅花形系统统计方法采集土壤样品。已将该性能与使用独立的高效液相色谱-电喷雾电离-（大气压化学电离-）串联质谱分析获得的相应统计变量进行了比较。
