摘要
以自制的敌百虫-D6为内标,采用均匀设计的实验方法优化固相萃取条件,建立了土壤中敌百虫的高效液相色谱-串联四极杆质谱的测定方法。本方法的前处理采用GCB/NH2固相萃取柱,以V（乙腈）∶V（甲苯）=3∶1为洗脱剂、丙酮为提取液,以Thermo Hypersil GOLD色谱柱为分离柱、V（甲醇）∶V（0.1%甲酸水溶液）=80∶20为流动相,并在电喷雾正离子的选择反应监测模式下进行检测。本方法的检出限为0.05 mg/kg,线性范围为0.1-10μg/m L,加标回收率为96.0%-103.8%,相对标准偏差（RSD）为1.0%～2.7%。
A method for the determination of pesticides residues in soil was developed by liquid chromatography-tandem mass spectrometry（LC-MS） with self-prepared trichlorfon-D6 as internal standard,and the conditions of solid phase extraction was optimized via uniform design.The sample pretreatment adopted GCB/NH2 solid phase extraction cartridge with V（acetonitrile） ∶V（methylbenzene） = 3 ∶1 as eluent,acetone as extractant.Chromatographic separation was carried out using the Thermo Hypersil GOLD separation column with the mobile phase of V（methyl alcohol） ∶ V（0.1% formic acid water solution） = 80 ∶ 20 and determined in the positive mode of SRM.The limit of detection was 0.05 mg/kg with the linear range 0.1 -10 μg/m L,recovery rates96.0% -103.8%,and RSD 1.0% ～ 2.7%.
出处
《化学试剂》
CAS
北大核心
2018年第1期49-52,88,共5页
Chemical Reagents
基金
科技部科技支撑计划项目(2015BAK45B01)
