顶空固相微萃取-气相色谱法测定生活饮用水中痕量1,4-二氧六环

发布时间：2018-07-17 02:58

【摘要】：建立了生活饮用水中痕量1,4-二氧六环的顶空固相微萃取(HS/SPME)-气相色谱测定方法。考察并优化了萃取头、萃取温度、萃取时间、pH值、样品量、色谱条件等参数。结果表明:提取效率较好的方法是3 mL水样中加入3 mL600 g/L氢氧化钠溶液,用85μm Carboxen-PDMS萃取头萃取,用键合碱改性的大口径、厚液膜PTA-5毛细管色谱柱测定。1,4-二氧六环在0.50~50.0μg/L范围内线性关系良好,相关系数为0.999 5;方法检出限(以S/N3计)为0.14μg/L;相对标准偏差为2.1%~4.5%(n=6);对实际样品中进行线性范围内的高、中、低3个加标水平的测定,回收率为95.5%~107%,相对标准偏差为1.1%~5.3%(n=6)。建立的方法简便、准确、重现性好、灵敏度高,适合生活饮用水中痕量1,4-二氧六环的常规监测。
[Abstract]:A headspace solid phase microextraction (HS- / SPME)-gas chromatographic method for the determination of trace 1 + 4-dioxane in drinking water was established. The parameters such as extraction head, extraction temperature, extraction time, pH value, sample quantity and chromatographic conditions were investigated and optimized. The results showed that the best extraction efficiency was the addition of 3 mL 600 g / L sodium hydroxide solution to the water sample, the extraction with 85 渭 m Carboxen-PDMS head, and the modification of large caliber by bonding base. PTA-5 capillary column with thick liquid membrane has a good linearity in the range of 0.50 ~ 50.0 渭 g / L, the correlation coefficient is 0.999; the detection limit (S / N _ 3) is 0.14 渭 g / L; the relative standard deviation is 2.1% (n ~ (6); The recoveries were 95. 5% and the relative standard deviations were 1. 1% and 5. 3% respectively. The method is simple, accurate, reproducible and sensitive. It is suitable for routine monitoring of trace 1 ~ 4 dioxane in drinking water.
【作者单位】：宁波市疾病预防控制中心浙江省微量有毒化学物健康风险评估技术研究重点实验室宁波市毒物研究与控制重点实验室;
【基金】：浙江省微量有毒化学物健康风险评估技术研究重点实验室建设项目(2013E10017)
【分类号】：O657.71;R123.1

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