水体与底泥中有机氯和除草剂农药残留的气相色谱串联质谱同步测定方法

发布时间：2018-08-29 16:33

【摘要】：本研究建立了水体和底泥中8种有机氯农药和5种除草剂的气相色谱-串联质谱(GC-MS/MS)同步测定分析方法.水样以甲醇作为基体改进剂,利用官能化聚苯乙烯/二乙烯苯(PEP)固相萃取柱富集和净化;底泥样品加乙腈用超声波辅助提取,二氯甲烷反萃取,使用氟罗里硅土固相萃取柱净化.采用DB-5MS(30 m×0.25 mm×0.25μm)色谱柱对待测物进行分离,多反应监测模式(MRM)测定.方法的线性相关性均大于0.999.空白水样在低、中、高等3个加标水平下的平均回收率为71%—115%,相对标准偏差(RSD)为4.0%—12.6%,检出限(LOD)0.12—2.0 ng·L~(-1).底泥样品在低、中、高等3个加标水平下,平均回收率为73%—120%,RSD为4.1%—11.0%,检出限(LOD)0.011—0.20μg·kg~(-1).该方法选择性好、灵敏度高且准确可靠,适合于水体和底泥中常见有机氯农药和除草剂类农药的检测.应用该方法测定了东北地区养殖池塘及松花江的水体和底泥样品.结果表明,莠去津检出率最高(100%),水体中残留量在11.2—1671 ng·L~(-1)之间,底泥中残留量在0.35—21.8μg·kg~(-1)之间.有机氯β-六六六检出率80%,水体中残留量在ND—6.76 ng·L~(-1)之间,底泥中残留量在ND—4.74μg·kg~(-1)之间.底泥样品中滴滴涕农药的残留量未超过我国淡水养殖产地环境限量标准.
[Abstract]:A method for simultaneous determination of 8 organochlorine pesticides and 5 herbicides in water and sediment by gas chromatography-tandem mass spectrometry (GC-MS/MS) was developed. Using methanol as matrix modifier, the water sample was enriched and purified by functionalized polystyrene / divinylbenzene (PEP) solid-phase extraction column, the sediment sample was extracted by ultrasonic assisted extraction with acetonitrile, and the dichloromethane was backextracted. A solid phase extraction column was used for purification of florolitic silica. The samples were separated by DB-5MS (30 m 脳 0.25 mm 脳 0.25 渭 m) column and determined by multi-reaction monitoring mode (MRM). The linear correlation of the method was higher than that of 0.999. The average recoveries of blank water samples were 71-115 at three higher standard levels, and the relative standard deviation (RSD) was 4.0-12.6.The detection limit of (LOD) was 0.12-2.0 ng L ~ (-1). The average recovery of sediment samples was 4.1- 11.0 at the three additional standard levels, the average recovery was 73-120, and the detection limit was 0.011-0.20 渭 g kg~ (-1). The method has the advantages of good selectivity, high sensitivity and high accuracy and reliability. It is suitable for the detection of common organochlorine pesticides and herbicides in water and sediment. This method was used to determine the water body and sediment samples of culture ponds and Songhua River in Northeast China. The results showed that the detection rate of atrazine was the highest (100%), the residue in water was between 11.2-1671 ng L-1 and the residue in sediment was between 0.35-21.8 渭 g kg~ (-1). The detectable rate of organochlorine 尾 -hexachloro-hexane was 80. The residual amount in water was between ND-6.76 ng L ~ (-1) and that in sediment was between ND-4.74 渭 g kg~ (-1). The residue of DDT pesticide in sediment samples did not exceed the environmental limit standard of freshwater breeding area in China.
【作者单位】：中国水产科学研究院黑龙江水产研究所;农业部水产品质量安全控制重点实验室;
【基金】：公益性行业(农业)科研专项(201503108) 中央级公益性科研院所基本科研业务费专项(HSY2016008)资助~~
【分类号】：X830

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