气相色谱-质谱联用法测定水源水中酞酸酯和己二酸酯

Determination of phthalate and adipate esters in the source water by solid-phase extraction and gas chromatography-mass detector

用C18固相萃取和液液萃取两种前处理方法处理水样,然后用气相色谱质谱联用(GCMS)定量测定水源水中的6种酞酸酯和己二酸二(2乙基己基)酯。研究结果表明,用C18固相萃取法测定目标化合物的加标回收率范围为65%～101%,相对标准偏差为5.50%～19.71%;用液液萃取法测定目标化合物的加标回收率范围为54.5%～107.6%,相对标准偏差为3.56%～14.47%。还研究了C18固相萃取法的方法检测限。除邻苯二甲酸二正丁酯的检测限为1.36μg/L外,其他目标化合物的检测限为0.05～0.48μg/L。该方法适用于监测水源水中6种酞酸酯和己二酸二(2乙基己基)酯。对实验过程中污染源的分析结果表明,固相萃取小柱、无水硫酸钠、玻璃毛和溶剂都有可能造成酞酸酯分析污染。

The present article intends to introduce the authors＇ method for determining the phthalate and adipate esters in the source water by solid-phase extraction and gas chromatography-mass detector. As we know, phthalate esters and bis（2-ethylhexyl） adipate ester have been widely used in recent years as plastieizers in many products for daily necessity, such as plasticizers, pesticides, paints and cosmetics, etc. They can also be leached from the above mentioned products and find a way to various enviromnental situations, thus bringing about the environmental contamination and threatening human health. Likely to be carcinogenic and estrogenic materials, such materials have to be dealt with seriously. So far, however, few papers have found to report the studies in this way at home, though a few reports can be found in analyzing phthalate esters and adipate esters by using GC-MS. This article has undertaken the experimental study in determining phthalate and adipate esters by GC-MS and have done two preparatory treatments （C18 solid-phase extraction and liquid-liquid extraction）, which is inclined to mean recovery of the solid phase extraction method from 65% to 101%. The range of the standard diversity proves from 5.50% to 19.71% while the mean recovery of the liquid-liquid extraction method is from 54.5% to 107.6% with the range of their standard diversity being from 3,56% to 14.47%. In addition, it is found that its limited detection is from 0.05 μg,/L to 0.48μg,/L except di-n-butyl phthalate ester, of which the detectable limit was 1.36 μg,/L. From the above results, it can be said that the method can be applied to determine the phthalate and adipate esters in some source water by C18 solid-phase extraction and GC-MS was applied. Besides, since the determination of phthalate and adipate esters may involve some kind of interference during the experiment, which might be caused by the solvent, glass wool, sodium sulfate and solid-phase extraction cartridge.