赵亚萌, 赵丹阳, 王翔, 赵忠林, 王霞. 固相萃取-气质联用测定饮用水中七类半挥发性有机物[J]. 环境与职业医学, 2018, 35(7): 654-660. DOI: 10.13213/j.cnki.jeom.2018.18315
引用本文: 赵亚萌, 赵丹阳, 王翔, 赵忠林, 王霞. 固相萃取-气质联用测定饮用水中七类半挥发性有机物[J]. 环境与职业医学, 2018, 35(7): 654-660. DOI: 10.13213/j.cnki.jeom.2018.18315
ZHAO Ya-meng, ZHAO Dan-yang, WANG Xiang, ZHAO Zhong-lin, WANG Xia. Determination of seven categories of semi-volatile organic chemicals in drinking water by solid-phase extraction and gas chromatography-mass spectrometry[J]. Journal of Environmental and Occupational Medicine, 2018, 35(7): 654-660. DOI: 10.13213/j.cnki.jeom.2018.18315
Citation: ZHAO Ya-meng, ZHAO Dan-yang, WANG Xiang, ZHAO Zhong-lin, WANG Xia. Determination of seven categories of semi-volatile organic chemicals in drinking water by solid-phase extraction and gas chromatography-mass spectrometry[J]. Journal of Environmental and Occupational Medicine, 2018, 35(7): 654-660. DOI: 10.13213/j.cnki.jeom.2018.18315

固相萃取-气质联用测定饮用水中七类半挥发性有机物

Determination of seven categories of semi-volatile organic chemicals in drinking water by solid-phase extraction and gas chromatography-mass spectrometry

  • 摘要: 目的 优化固相萃取-气质联用测定饮用水中七类半挥发性有机物的方法。

    方法 40 L水样分别经不同固相萃取方式(XAD-2单柱,XAD-2与活性炭双柱串联)进行有机物富集,XAD-2萃取剂依次经甲醇:丙酮(7:3)、丙酮:正己烷(1:1)、二氯甲烷洗脱;活性炭依次经丙酮:正己烷(1:1)、二氯甲烷洗脱。待洗脱液自然挥干,甲醇复溶,内标法定量,气相色谱-质谱联用检测。

    结果 本方法各物质色谱峰分离度较好,七类物质在0.05~5 μg/mL浓度范围内线性良好。双柱萃取提高了115种化学物的回收率。有机氯农药、有机氮农药、多氯联苯、邻苯二甲酸酯和高分子量多环芳烃回收率大多在70%~110%,精密度在20%以下。大多数亚硝胺类和高挥发性酚类回收率较低。方法检出限能够满足饮用水水样检测的需要。

    结论 本研究XAD-2与活性炭串联萃取效果优于XAD-2单柱萃取,优化的水中七类半挥发性有机物的固相萃取-气质联用法较为灵敏,适合于大体积饮用水样的富集检测。

     

    Abstract: Objective To modify a method combining solid-phase extraction (SPE) and gas chromatography-mass spectrometry (GC-MS) to determine seven categories of semi-volatile organic chemicals in drinking water.

    Methods Water samples (40 L) were extracted by different SPE columns (XAD-2 column, XAD-2/activated carbon tandem columns). XAD-2 was eluted with methanol:acetone (7:3), acetone:hexane (1:1), and dichloromethane in sequence. Activated carbon was eluted with acetone:hexane (1:1) and dichloromethane in sequence. The eluents were dried in air and dissolved in methanol. The concentrations of semi-volatile organic chemicals were determined by GC-MS with internal standard method.

    Results The chromatographic peak resolution of the proposed detection method was good, and the linearities of the seven categories of chemicals were good within the range of 0.05-5 μg/mL. The recoveries of 115 chemicals using XAD-2/activated carbon tandem columns were improved. The recoveries of organochlorine pesticides, organonitrogen pesticides, polychlorinated biphenyls, phthalate esters, and high-molecular-weight polycyclic aromatic hydrocarbons were mostly in the range of 70%-110%, and the precisions were below 20%. The recoveries of most nitrosamines and high volatile phenols were low. The method's detection limits satisfied the detection requirements of drinking water.

    Conclusion The enrichment efficiency of XAD-2/activated carbon tandem columns is higher than that of XAD-2 column alone. The modified SPE-GC-MS method is sensitive for determination of seven categories of semi-volatile organic chemicals in drinking water, and is suitable for the enrichment and detection of large-volume drinking water samples.

     

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