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    离子色谱-质谱法快速测定橡胶制品产业园周边土壤中6种污染物的残留量

    Rapid Determination of Residues of 6 Pollutants in Soil around Rubber Products Industrial Park by Ion Chromatography-Mass Spectrometry

    • 摘要: 提出了离子色谱-质谱法(IC-MS)快速测定橡胶制品产业园周边土壤中丁基黄原酸、二氯乙酸、三氯乙酸、没食子酸、酒石酸、对香豆酸等6种污染物残留量的方法。取风干并过筛后的土壤样品10 g置于萃取池中,加入20 g硅藻土,以体积比2∶1的甲醇-丙酮混合溶液进行加速溶剂萃取,萃取液经0.22 μm聚醚砜滤膜过滤,采用IC-MS测定6种污染物的含量。以DIONEX Ion-Pac AS17色谱柱为固定相,以0.1 mol·L−1氢氧化钾溶液为淋洗液分离6种污染物,质谱分析采用电喷雾离子(ESI)源,在负离子(ESI)扫描模式下采用多反应监测(MRM)模式检测。结果表明,6种污染物的质量浓度在0.005~5.0 mg·L−1内与对应的峰面积呈线性关系,检出限(3S/N)为0.009~0.023 μg·L−1;按照标准加入法进行回收试验,回收率为83.8%~95.1%,测定值的相对标准偏差(n=6)均小于5.0%;方法用于测定实际橡胶制品产业园周边土壤样品中6种污染物的残留量,其中酒石酸未检出,其余污染物的检出量为13.04~61.25 µg·L−1

       

      Abstract: A method for rapid determination of residues of 6 pollutants including butyl xanthan acid, dichloroacetic acid, trichloroacetic acid, gallic acid, tartaric acid, and p-coumaric acid in soil around rubber products industrial park by ion chromatography-mass spectrometry (IC-MS) was proposed. 10 g of the dried and sieved soil sample was taken, and placed in the extraction tank. 20 g of diatomite was added, and the mixture was extracted with a mixed solution of methanol and acetone at a volume ratio of 2∶1 by accelerated solvent extraction. The extract was passed through a 0.22 μm polyether sulfone filter membrane, in which 6 pollutants were determined by IC-MS. DIONEX Ion-Pac AS17 chromatographic column was used as the stationary phase, and 0.1 mol·L−1 potassium hydroxide solution was used as the rinsing solvent to separate the 6 pollutants. Electrospray ion (ESI) source was used for mass spectrometry. The targets were detected by multiple reaction monitoring (MRM) mode in negative ion (ESI) scanning mode. As shown by the results, linear relationships between the corresponding peak areas and mass concentrations of 6 pollutants were found within 0.005-5.0 mg·L−1, with detection limits (3S/N) in the range of 0.009-0.023 μg·L−1. Test for recovery was made by the standard addition method, giving results in the range of 83.8%-95.1%, with RSDs (n=6) of the determined values less than 5.0%. This method was used to determine the residues of 6 pollutants in actual soil samples around rubber products industrial park, tartaric acid was not detected, and the detected amounts of the other pollutants were in the range of 13.04-61.25 µg·L−1.

       

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