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基于整体材料的搅拌棒吸附萃取结合二极管阵列检测液相色谱法测定尿液基质中的甾体性激素。

Determination of steroid sex hormones in urine matrix by stir bar sorptive extraction based on monolithic material and liquid chromatography with diode array detection.

作者信息

Huang Xiaojia, Yuan Dongxing, Huang Benli

机构信息

State Key Laboratory of Marine Environmental Science, Environmental Science Research Center, Xiamen University, Xiamen 361005, China.

出版信息

Talanta. 2008 Mar 15;75(1):172-7. doi: 10.1016/j.talanta.2007.10.052. Epub 2007 Nov 9.

Abstract

A simple, rapid and sensitive method for simultaneous determination of six steroid sex hormones in urine matrix was developed by the combination of stir bar sorptive extraction (SBSE) with high performance liquid chromatography (HPLC) and diode array detection (DAD). A poly (methacrylic acid stearyl ester-ethylene dimethacrylate) was synthesized and selected as SBSE extraction medium. To achieve the optimum extraction performance, several parameters, including agitation speed, desorption solvent, extraction and desorption time, pH value, inorganic salt and organic solvent content of the sample matrix were investigated. Under the optimized experimental conditions, low detection limits (S/N=3) and quantification limits (S/N=10) of the proposed method for the target compounds were achieved within the range of 0.062-0.38 and 0.20-1.20 ng/mL, respectively from spiked urine, respectively. The calibration curves of six steroid sex hormones showed good linearity ranging from 1.0 to 200 ng/mL with linear coefficient R2 values above 0.990. Good method reproducibilities presented as intra- and inter-day precisions were also found with the R.S.D.s less than 9.2 and 10.0%, respectively. Finally, the proposed method was successfully applied to the determination of the target compounds in a urine sample from a pregnant woman.

摘要

通过搅拌棒吸附萃取(SBSE)与高效液相色谱(HPLC)及二极管阵列检测(DAD)相结合,开发了一种用于同时测定尿液基质中六种甾体性激素的简单、快速且灵敏的方法。合成了聚(甲基丙烯酸硬脂酯 - 二甲基丙烯酸乙二酯)并将其选作SBSE萃取介质。为实现最佳萃取性能,研究了几个参数,包括搅拌速度、解吸溶剂、萃取和解吸时间、pH值、样品基质中的无机盐和有机溶剂含量。在优化的实验条件下,该方法对加标尿液中目标化合物的检测限(S/N = 3)和定量限(S/N = 10)分别在0.062 - 0.38 ng/mL和0.20 - 1.20 ng/mL范围内。六种甾体性激素的校准曲线在1.0至200 ng/mL范围内呈现良好线性,线性系数R2值高于0.990。日内和日间精密度表示的方法重现性也很好,相对标准偏差分别小于9.2%和10.0%。最后,该方法成功应用于一名孕妇尿液样品中目标化合物的测定。

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