Specific determination of linear Alkylbenzenesulfonates (LAS) in commercial detergents and whole blood by high-performance liquid chromatography with solid-phase extraction.
Specific determination of linear Alkylbenzenesulfonates (LAS) in commercial detergents and whole blood by high-performance liquid chromatography with solid-phase extraction.
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DOI：
10.1093/jat/31.1.37
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发表时间：
2007
影响因子：
2.5
通讯作者：
Y. Xue;Y. Hieda;J. Fujihara;K. Takayama;H. Takeshita
中科院分区：
文献类型：
--
作者：
Y. Xue;Y. Hieda;J. Fujihara;K. Takayama;H. Takeshita
本文采用固相萃取（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）。样品用萃取液缓冲，用Bakerbond C（18）SPE柱纯化。将柱洗涤、干燥，并用实验优化的溶剂系统洗脱。使用Wakopak WS AS-Aqua柱（4.6 * 250-mm）进行HPLC，并使用UV检测器在228 nm处监测。采用由乙腈/水（60：40，v/v）组成并含有1.2%（w/v）高氯酸钠的移动的流动相。在6.85和13.79 min洗脱的LAS的五种同系物（C（10）约C（14））实现了良好的分离。发现该分析的线性范围为10.0 - 100.0 ng/g，检测限为4.0-5.0 ng/g。血液中各同系物的回收率范围为76 - 107%。用该方法可以提取洗涤剂中的LAS，并检测出C（10）与C（13）的同系物。用本方法测定了口服市售洗涤剂的大鼠血样，并将C（14）用作内标。该方法简便、可靠，适用于法医学和临床标本中LAS的测定。
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.