土壤和大米中得克隆检测方法的研究

Study on the detection method of dechlorane plus residue in soil and rice

为探究对高氯代阻燃剂得克隆选择性好和灵敏度高的检测方法,采用振荡提取和加速溶剂萃取(ASE)两种方法对土壤和大米中得克隆的两种异构体残留进行提取,利用TSQ 8000三重四极杆GC-MS/MS(气相色谱质谱/质谱联用)的二级质谱检测分析,建立了土壤和大米中得克隆的残留测定方法。结果表明,得克隆的两种同分异构体syn-DP和anti-DP在试验测定条件下保留时间比较合适,线性范围分别为5.00×10^-13~4.02×10^-9g和1.62×10^-12~1.30×10^-8g,最低检出限分别为1.00×10^-13g和5.0×10^-14g。对于土壤样品中的syn-DP,在试验设定的添加浓度下,振荡提取和ASE方法添加回收率分别为85.32%~91.42%和90.69%~95.63%,变异系数均小于4.64%;对于anti-DP,振荡提取和ASE方法添加回收率分别为82.45%~90.16%和88.78%~98.23%,变异系数均小于4.96%。采用ASE法,大米中syn-DP和anti-DP的回收率分别为90.56%~98.56%和90.36%~96.56%,变异系数均小于5.05%,振荡提取法回收率小于加速溶剂萃取法,分别为86.47%~90.24%和85.84%~89.61%,变异系数均小于4.53%,达到了痕量syn-DP和anti-DP残留分析方法的要求。研究表明,采用ASE和振荡提取两种预处理样品的方法,二者的回收率均能满足土壤和大米样品中得克隆的痕量残留检测分析方法的要求,且该分析方法灵敏度高、准确性好,适合土壤和大米中得克隆的残留检测。

To explore the methodology of determination of high chlorinated flame retardant dechlorane plus(DP)with good selection and high sensitivity,oscillation extraction and accelerated solvent extraction(ASE)were used to extract the residues of two isomers from soil and rice.The DP in the extracted residue from soil and rice was analyzed and detected by TSQ 8000 triple quadrupole rod gas chromatography-mass spectrometry(GC-MS)/mass spectrometry(MS).The results showed that the retention time of the syn-DP and anti-DP was suitable for the determination,with the linear range of 5.00×10−13~4.02×10−9 g and 1.62×10−12~1.30×10−8 g and the lowest detection limit of 1.00×10−13 g and 5.0×10−14 g.For syn-DP in soil samples,the recovery rates of oscillatory extraction and ASE method were 85.32%~91.42%and 90.69%~95.63%,respectively,and the coefficients of variation were less than 4.64%.For anti-DP,the recovery rates of oscillatory extraction and ASE method were 82.45%~90.16%,and 88.78%~98.23%,respectively,and the coefficients of variation were less than 4.96%.The recovery of ASE of syn-DP and anti-DP in rice was 90.56%~98.56%and 90.36%~96.56%,respectively,the coefficient of variation was less than 5.05%,and the recovery of oscillatory extraction was 86.47%~90.24%and 85.84%~89.61%,respectively,and the coefficient of variation was less than 4.53%,meeting the requirements of trace syn-DP and anti-DP residue analysis.In this study,the recovery rates of both ASE and oscillation extraction of two different pretreatment samples could meet the requirements of the trace residue detection and analysis method of DP obtained from soil and rice samples,which is sensitive,accurate,and suitable for the residue detection of DP obtained from soil and rice.It is important to establish a method for the determination of trace DP in soil and rice by GC-MS/MS.