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作 者:薛玉英[1,2] 张姗姗[1] 唐萌[1] 稗田洋子 竹下治男
机构地区:[1]东南大学公共卫生学院,南京210009 [2]岛根大学医学院,岛根6938501
出 处:《理化检验(化学分册)》2010年第1期25-27,31,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基 金:日本学术振兴会特别研究员奖励费(17.05226);国家重点基础研究发展计划(973计划)课题(2006CB705602);国家自然科学基金项目(30671782)
摘 要:提出了高效液相色谱法测定全血中直链烷基苯磺酸钠同系物的含量。全血样品用酸性提取溶液稀释,过Bakerbond SPE C18固相萃取小柱,经甲醇-乙酸-水(49+2+49)混合溶液淋洗后用甲醇-氨水(98+2)混合溶液洗脱。经纯化后的洗脱液在Wakopak WS AS-Aqua(250 mm×4.6 mm,5 μm)柱上进行分离,流动相为乙腈与水(60+40)混合溶液,检测波长为228 nm。5种n-ABS同系物的C10-C14的质量分数在10.0-100.0 ng·g-1范围内与其峰面积呈线性关系,全血中各同系物回收率为78%-107%;日内相对标准偏差(n=5)≤10%,日间相对标准偏差(n=5)≤13%。A method for the determination of homologues of n-alkylbenzenesulfonates in whole blood by high- performance liquid chromatography (HPLC) was proposed. The sample of whole blood was diluted with an acidic extractant and purified on the Bakerbond C18 SPE column. The column was first rinsed with a mixed solution of CH3OH+HOAc+H20 (49+2+49) and then eluted with mixed solution of CH3OH and aqueous ammonia (98+ 2). The homologues of n-ABS were separated on Wakopak WS AS-Aqua column (250 mm×4. 6 mm, 5 μm) with mixed solution of acetonitrile and water (60+40) as mobile phase, and determined with UV-detection at 228 nm. Linearity ranges for 5 C10 -C14 homologues of n-ABS was found ranged from 10. 0 to 100. 0 ng . g-1 and values of recovery of the 5 homologues in whole blood ranged from 78% to 107% were obtained. Values of intraday and interday RSDrs (n=5) were less than 10% and 13%, respectively.
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