摘要
目的建立饮用水中24种半挥发有机污染物(SVOCs)的大体积固相萃取-气相色谱-质谱(GC-MS)快速同时测定方法。方法水样加入抗坏血酸后,在酸性条件(pH<2)下,以15 ml/min通过大容量聚合物固相萃取柱连续吸附、富集后,依次用3 ml乙酸乙酯、3 ml二氯甲烷和1.5 ml甲醇洗脱,洗脱液经无水硫酸钠脱水、氮吹浓缩后用乙酸乙酯定容至1 ml,采用GC-MS进行检测,内标法定量。结果在0.1~2.0μg/L的线性范围内,所得24种SVOCs的回归方程均呈较好的线性关系(r>0.992)。该方法的检出限为0.006~0.068μg/L,定量下限为0.020~0.397μg/L,平均回收率为62.9%~117.4%,RSD<10%。结论该方法可有效提取、富集、浓缩和净化大体积水样,一次进样,同时分离和测定多种半挥发有机物,操作简单、准确灵敏,适合于大体积水样中24种痕量SVOCs的同时快速检测。
Objective To develop a rapid method of the simuhaneous determination of 24 semi-volatile organic compounds （SVOCs） in drinking water by high capacity solid phase extraction and gas chromatography-mass spectrometry. Methods Ascorbic acid was added into water samples. At acidic conditions （pH〈2）, water sample was extracted through the high-capacity polymer solid phase extraction column at 15 ml/min flow rate. After continuous adsorption,enrichment,washing with 3 ml of ethyl acetate, 3 ml dichloro-methane and 1.5 ml methanol eluate , dehydration by anhydrous sodium sulfate, concentration by nitrogen blowing ,the concentrate was concentrated to 1 ml with ethyl acetate,then were detected by GC-MS, quantitatively analyzed with internal standard method. Results In the linear range of 0.1-2.0 p^g/L,the regression equation showed a good linear correlation,r〉0.992. The detection limits of the method for 24 kinds of SVOCs were 0.006-0.068 p,g/L, the limits of quantification were 0.020-0.397 p.g/L,the average recoveries were 62.9%-l17.4%,RSDs〈lO%. Conclusion This method can extract,enrich,concentrate and purify the bulk water samples,with the advantage of a single injection,the simultaneous separation and determination of a variety of semi-volatile organic compounds, and it is simple,accurate and sensitive and suitable for large volume of trace 24 kinds of SVOCs meanwhile rapid detection.
出处
《环境与健康杂志》
CAS
CSCD
北大核心
2013年第9期805-809,共5页
Journal of Environment and Health
基金
卫生部卫生标准制(修)订项目(20110101-5)
广东省医学科研基金(B2010027
B2012021)
广东省自然科学基金(S2012010009877)
关键词
大体积固相萃取
色谱法
气相
质谱法
半挥发性有机物
饮用水
High capacity solid phase extraction
Chromatography, gas
Mass spectrometry
Semi-volatile organic compounds
Drinking water
