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    加速溶剂萃取联合凝胶色谱净化-气相色谱-质谱法测定土壤中21种酚类化合物的含量

    Determination of 21 Phenolic Compounds in Soil by Gas Chromatography-Mass Spectrometry after Accelerated Solvent Extraction Combined with Gel Chromatography Purification

    • 摘要: 提出了加速溶剂萃取联合凝胶色谱净化-气相色谱-质谱法同时测定土壤中21种酚类化合物含量的方法。取研细过筛后的土壤样品(含水率15%~20%)10 g,加入6 g硅藻土混匀并研磨,置于萃取罐中,以体积比2∶1的二氯甲烷-正己烷混合溶液于120 ℃进行加速溶剂萃取,萃取液经无水硫酸钠脱水,再用二氯甲烷充分淋洗无水硫酸钠,合并全部有机相,浓缩至1 mL,通过凝胶色谱进行净化,收集9~18 min的流出液,浓缩至1 mL,在HP-5MS色谱柱上按照柱升温程序分离,质谱分析采用全扫描(SCAN)模式。结果表明,21种酚类化合物的质量浓度在2.50~50.0 mg·L−1内与对应的峰面积呈线性关系,检出限(3.143s)为0.02~0.07 mg·kg−1。按照标准加入法进行回收试验,回收率为73.4%~107%,测定值的相对标准偏差(n=6)均不大于17%。方法用于2份土壤样品分析,21种酚类化合物均未检出。方法用于土壤质控样品分析,21种酚类化合物的测定值均在认定值的不确定度范围内。

       

      Abstract: A method for simultaneous determination of 21 phenolic compounds in soil by gas chromatography-mass spectrometry after accelerated solvent extraction combined with gel chromatography purification was proposed. 10 g of the finely sieved soil sample (moisture content of 15%-20%) was taken, and 6 g of diatomite was added. The mixture was mixed uniform and placed in the extraction tank, extracted with a mixed solution of dichloromethane and n-hexane at the volume ratio of 2∶1 at 120 ℃ by accelerated solvent extraction. Anhydrous sodium sulfate was used to dehydrate the extract, and then thoroughly rinsed with dichloromethane. All organic phases were combined and concentrated to 1 mL. The concentrated solution was purified by gel chromatography, and the effluent of 9-18 min was collected, then concentrated to 1 mL. The 21 phenolic compounds in the solution were separated on a HP-5MS column according to the column heating program, and SCAN mode was adopted in mass spectrometry analysis. As shown by the results, linear relationships between the corresponding peak areas and mass concentrations of 21 phenolic compounds were found in the range of 2.50-50.0 mg·L−1, with detection limits (3.143s) in the range of 0.02-0.07 mg·kg−1. Test for recovery was made by the standard addition method, giving results in the range of 73.4%-107%, with RSDs (n=6) of the determined values not more than 17%. This method was used for the analysis of 2 soil samples, and 21 phenolic compounds were not detected. This method was used for the analysis of soil quality control sample, and the determined values of 21 phenolic compounds were all within the uncertainty ranges of the certified values.

       

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