Xue Yuying, Hieda Yoko, Fujihara Junko, Takayama Koji, Takeshita Haruo
Department of Legal Medicine, Shimane University Faculty of Medicine, 89-1 Enya, Izumo, Shimane 693-8501, Japan.
J Anal Toxicol. 2007 Jan-Feb;31(1):37-43. doi: 10.1093/jat/31.1.37.
This paper presents the extraction and analysis of linear alkylbenzenesulfonates (LAS) from whole blood using solid-phase extraction (SPE) together with high-performance liquid chromatography (HPLC). The sample was buffered with extraction solution and purified with Bakerbond C(18) SPE columns. The columns were washed, dried, and eluted with experimental optimized solvent systems. HPLC was performed using a Wakopak) WS AS-Aqua column (4.6 * 250-mm) and monitored at 228 nm using a UV detector. A mobile phase consisting of acetonitrile/water (60:40, v/v) and containing 1.2% (w/v) of sodium perchlorate was employed. Good separation was achieved for the five homologues of LAS (C(10) approximately C(14)) eluted at 6.85 and 13.79 min. The linearity range for this analysis was found to be from 10.0 to 100.0 ng/g and the limit of detection was 4.0-5.0 ng/g in blood for each homologue. The recovery of each homologue in blood ranged from 76 to 107%. The LAS in commercial detergents could be extracted and the homologues of C(10) approximately C(13) were detected. Blood samples of rats, which were administered a commercial detergent orally, were determined by the present method, and C(14) was used as an internal standard. The method was simple and reliable for the determination of LAS in blood samples and could be expected to apply to the forensic and clinical specimens.
本文介绍了采用固相萃取(SPE)结合高效液相色谱(HPLC)从全血中提取和分析直链烷基苯磺酸盐(LAS)的方法。样品用萃取溶液缓冲,并用Bakerbond C(18)固相萃取柱纯化。柱子经洗涤、干燥后,用实验优化的溶剂系统洗脱。HPLC使用Wakopak WS AS-Aqua柱(4.6×250 mm)进行,用紫外检测器在228 nm处监测。采用由乙腈/水(60:40,v/v)组成且含有1.2%(w/v)高氯酸钠的流动相。LAS的五个同系物(C(10)至C(14))在6.85和13.79分钟洗脱时实现了良好分离。该分析的线性范围为10.0至100.0 ng/g,每个同系物在血液中的检测限为4.0 - 5.0 ng/g。每个同系物在血液中的回收率为76%至107%。可以从商用洗涤剂中提取LAS,并检测到C(10)至C(13)的同系物。采用本方法测定经口给予商用洗涤剂的大鼠血液样本,以C(14)作为内标。该方法用于测定血液样本中的LAS简单可靠,有望应用于法医和临床样本。