竹炭固相萃取/气相色谱-质谱联用对环境水样中16种多环芳烃的测定  

Determination of 16 PAHs in Water Samples by Solid-phase Extraction Using Bamboo Charcoal as the Absorbent Coupled with GC-MS

作　　者：肖荣辉[1] 马继平[1] 鹿文慧[1] 史本章[1] 吕丽莉[1] 李茉[1] 

机构地区：[1]青岛理工大学环境与市政工程学院,山东青岛266033

出　　处：《分析测试学报》2009年第9期1022-1026,共5页Journal of Instrumental Analysis

基　　金：山东省教育厅科技计划项目资助(J07WZ05);青岛理工大学引进人才科研启动基金资助项目(C2007-008);山东省教育厅高等学校优秀骨干教师国际合作培养项目资助

摘　　要：以竹炭为固相萃取吸附材料,考察了其对环境水样中16种多环芳烃的吸附富集能力,采用DB-35MS弹性石英毛细管色谱柱对16种多环芳烃进行分离,气相色谱-质谱联用法对多环芳烃进行定性及定量分析。结果表明,1000mg竹炭作为固相萃取吸附剂,10mL二氯甲烷作为洗脱剂,上样速率5mL/min,水样中甲醇体积分数为15%的条件下,16种多环芳烃有较好的回收率,竹炭固相萃取柱的穿透体积大于500mL,通过实验比较竹炭的萃取回收率优于商品化的C18固相萃取柱。16种多环芳烃的质量浓度在10～500ng/L范围内与峰面积的线性关系良好(苯并(k)荧蒽,苯并(a)芘,二苯并(a,h)蒽,苯并(g,h,i)苝为25～500ng/L),相关系数为0.9836～0.9984。方法的检出限为0.6～8.0ng/L,实际水样的加标回收率为67%～113%,相对标准偏差为2.1%～11.3%。通过对白沙河河水的分析表明,该方法能够满足实际水样的测定,竹炭可以作为固相萃取材料应用于水中16种多环芳烃的分析测定。A solid-phase extraction （SPE） using bamboo charcoal as absorbent coupled with gas chro- matography- mass spectrometry（ GC -MS） analytical method was developed for the determination of 16 polycyclic aromatic hydrocarbons （PAHs） in environmental water samples. In this paper, 16 PAHs were separated successfully by DB-35MS capillary chromatographic column. The effect of ex- perimental parameters, such as flow rate of sample loading, type and volume of eluent, and concen- tration of organic solvent on extraction efficiency were optimized. A good extraction efficiency was obtained by using 1 000 mg bamboo charcoal as SPE adsorbent and 10 mL dichloromethane as eluent with 5.0 mL/min of extract rate and 15% organic solvent（methanol） in the water sample. Compared with the commercial Cls SPE packing material, bamboo charcoal had higher recoveries for 16 PAHs. Under the optimal conditions, the results showed that excellent linearity was obtained over the range of 10 - 500 ng/L for PAHs except for benzol k] fluoranthene, benzol a] pyrene, dibenzo[ a, h] an- thracene, benzol g, h, i] perylene in the range of 25 -500 ng/L. Linear correlation coefficients （r2） varied between 0.983 6 and 0.998 4. Limits of detection（LODs） ranged from 0.6 to 8.0 ng/L. The proposed method was successfully applied to the analysis of river water sample. The spiked recoveries of 16 PAHs were in the range of 67% - 113% with RSDs of 2. 1% - 11.3%. The results showed the method was cheap, simple, and could used as an excellent alternative for the rou- tine analysis in environmental field.

关 键 词：竹炭 固相萃取 气相色谱-质谱法 多环芳烃 水样 

分 类 号：O657.7[理学—分析化学] TQ413.213[理学—化学]