Jia Lijuan, Deng Yunyun
Bioassay and Safety Assessment Lab, Shanghai Academy of Public Measurement, Shanghai 201203, China.
Se Pu. 2008 Nov;26(6):697-703.
A method was developed for the determination of organochlorine pesticides (OCPs) in soils using accelerated solvent extraction (ASE, Florisil cleanup in the extraction cell) and gel permeation chromatography (GPC) on-line concentration prior to the determination by ga chromatography-triple quadrupole tandem mass spectrometry (GC-MS/MS). And then 20 agricultural soil samples in Shanghai suburbs were determined. Multiple reaction monitoring (MRM) was applied to qualify and quantify the target compounds. In the different linear ranges (included in 0.001 - 0.2 mg/L) of each pesticide, the correlation coefficients were higher than 0.995. The average recoveries in spiked soils were 65.9% - 140.0% with the relative standard deviations of 1.5% - 20.3% (n = 5). The limits of detection (LOD) (S/N = 3) for these pesticides were from 0.1 to 3.0 microg/kg and the limits of quantification (LOQ) (S/N = 10)were from 0.3 to 8.0 microg/kg. Among these soils, hexachlorocyclohexane (HCHs) and hexachlorobenzene (HCB) were detected little with a content ranges of 1.82 - 3.70 and 0.94 -9.8 microg/kg, respectively. DDTs (including 2-(2-chlorophenyl)-2-(4-chloropenyl) -1,1,1-trichloroethane (p, p'-DDT), 2,2-bis (4-chlorophenyl)-1,1-dichloro-ethylene (p,p'-DDE), 2,2-bis (4-chlorophenyl)-1,1-dichloroethane (p,p'-DDD)) were found widely with a range of 1.08 - 308.76 microg/kg and mean value of 53.28 microg/kg. The content ratio of DDT/( DDE + DDD) were less than 1.0 in 85% soil samples, indicating that DDT might come from the early days.
建立了一种采用加速溶剂萃取（ASE，萃取池中使用弗罗里硅土净化）和凝胶渗透色谱（GPC）在线浓缩，然后通过气相色谱 - 三重四极杆串联质谱（GC-MS/MS）测定土壤中有机氯农药（OCPs）的方法。随后对上海郊区的20个农业土壤样品进行了测定。采用多反应监测（MRM）对目标化合物进行定性和定量。在每种农药的不同线性范围（0.001 - 0.2 mg/L）内，相关系数均高于0.995。加标土壤中的平均回收率为65.9% - 140.0%，相对标准偏差为1.5% - 20.3%（n = 5）。这些农药的检测限（LOD）（S/N = 3）为0.1至3.0 μg/kg，定量限（LOQ）（S/N = 10）为0.3至8.0 μg/kg。在这些土壤中，六氯环己烷（HCHs）和六氯苯（HCB）检出量很少，含量范围分别为1.82 - 3.70和0.94 - 9.8 μg/kg。滴滴涕（DDTs，包括2-(2-氯苯基)-2-(4-氯苯基)-1,1,1-三氯乙烷（p,p'-DDT）、2,2-双(4-氯苯基)-1,1-二氯乙烯（p,p'-DDE）、2,2-双(4-氯苯基)-1,1-二氯乙烷（p,p'-DDD））广泛存在，范围为1.08 - 308.76 μg/kg，平均值为53.28 μg/kg。85%的土壤样品中DDT/(DDE + DDD)的含量比小于1.0，表明DDT可能来自早期。
