Zhang Ming-quan, Li Feng-min, Wu Qian-yuan, Hu Hong-ying
College of Environmental Science and Engineering, Ocean University of China, Qingdao 266100, China.
Huan Jing Ke Xue. 2013 May;34(5):1851-6.
A concentration method for enrichment of toxic organic compounds in water samples has been developed based on combined solid-phase extraction (SPE) to reduce impurities and improve recoveries of target compounds. This SPE method was evaluated in every stage to identify the source of impurities. Based on the analysis of Waters Oasis HLB without water samples, the eluent of SPE sorbent after dichloromethane and acetone contributed 85% of impurities during SPE process. In order to reduce the impurities from SPE sorbent, soxhlet extraction of dichloromethane followed by acetone and lastly methanol was applied to the sorbents for 24 hours and the results had proven that impurities were reduced significantly. In addition to soxhlet extraction, six types of prevalent SPE sorbents were used to absorb 40 target compounds, the lgK(ow) values of which were within the range of 1.46 and 8.1, and recovery rates were compared. It was noticed and confirmed that Waters Oasis HLB had shown the best recovery results for most of the common testing samples among all three styrenedivinylbenzene (SDB) polymer sorbents, which were 77% on average. Furthermore, Waters SepPak AC-2 provided good recovery results for pesticides among three types of activated carbon sorbents and the average recovery rates reached 74%. Therefore, Waters Oasis HLB and Waters SepPak AC-2 were combined to obtain a better recovery and the average recovery rate for the tested 40 compounds of this new SPE method was 87%.
基于组合固相萃取（SPE）开发了一种富集水样中有毒有机化合物的浓缩方法，以减少杂质并提高目标化合物的回收率。对该SPE方法的每个阶段进行了评估，以确定杂质来源。通过对未添加水样的Waters Oasis HLB进行分析，发现二氯甲烷和丙酮洗脱后的SPE吸附剂洗脱液在SPE过程中贡献了85%的杂质。为了减少SPE吸附剂中的杂质，对吸附剂采用二氯甲烷、丙酮、最后是甲醇的索氏提取24小时，结果证明杂质显著减少。除了索氏提取外，还使用六种常见的SPE吸附剂吸附40种目标化合物，其lgK(ow)值在1.46至8.1范围内，并比较了回收率。注意到并证实，在所有三种苯乙烯-二乙烯基苯（SDB）聚合物吸附剂中，Waters Oasis HLB对大多数常见测试样品显示出最佳的回收率结果，平均为77%。此外，在三种活性炭吸附剂中，Waters SepPak AC-2对农药具有良好的回收率结果，平均回收率达到74%。因此，将Waters Oasis HLB和Waters SepPak AC-2结合起来以获得更好的回收率，这种新SPE方法对40种测试化合物的平均回收率为87%。
