气相色谱-串联质谱法测定滩涂生物样本中的六六六和滴滴涕

目的建立滩涂生物样本中的六六六(HCHs)和滴滴涕(DDTs)的气相色谱-串联质谱(GC-MS/MS)测定法。方法取可食部位匀浆样品加无水硫酸钠脱水、使用石油醚进行超声萃取,再加硫酸磺化后静置取有机相氮气吹干定容,取上清液经HP-5MS Ultra Inert毛细管气相色谱柱(30 m×250μm,0.25μm)分离,气相色谱-串联质谱分离检测,外标法定量。结果本法六六六和滴滴涕在0.100μg/L^10.0μg/L线性相关系数均≥0.999,方法检出限均为0.02μg/kg,平均样本加标回收率为57.6%~100%,相对标准偏差(RSD)在0.100μg/kg水平为15.1%~23.0%,1.00μg/kg水平为8.12%~17.1%,10.0μg/kg水平为3.22%~9.03%。使用本方法检测实际样品,六六六检出率为44.0%,滴滴涕检出率为99.0%,检出浓度为0.035μg/kg^8.17μg/kg。结论该方法前处理过程简便,定性及定量准确,灵敏度高,满足批量样品的检测。

Determination of HCHs and DDTs in tideland biological samples by gas chromatography-tandem mass spectrometry

Objective A gas chromatography-tandem mass spectrometry(GC-MS/MS) was established for the determination of HCHs and DDTs in tideland biological samples.Methods The edible parts of the sample were dehydrated with anhydrous sodium sulfate and ultrasonically extracted with petroleum ether.After sulfonated with sulfuric acid,the organic phase was blown-dried and the volume was fixed.The supernatant was separated by HP-5 MS Ultra Inert column(30 m × 250 μm,0.25 μm) and detected by GC-MS/MS and quantified by external standard method.Results In the range of 0.100 μg/L-10.0 μg/L,the correlation coefficients were ≥0.999,with the detection limits of 0.02 μg/kg,and the recoveries was within57.6%-100%.The RSD ranges were within 15.1%-23.0% at 0.100 μg/kg,8.12%-17.1% at 1.00 μg/kg and3.22%-9.03% at 10.0 μg/kg.The actual sample was detected by this method.The detection rate of BHC was 44.0%,the detection rate of DDT was 99.0%,and the detection contents ranged from 0.035 μg/kg to 8.17 μg/kg.Conclusion The method has the advantages of simple pretreatment,accurate qualitative and quantitative analysis,high sensitivity,and can be applied for the detection of HCHs and DDTs in batch samples.