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[高效液相色谱法测定人尿液中的异硫氰酸盐]

[Determination of isothiocyanates in human urine by high performance liquid chromatography].

作者信息

Chu Xingdi, Zhu Lifang, Gao Yutang

机构信息

Department of Epidemiology, Shanghai Cancer Institute, Shanghai 200032, China.

出版信息

Se Pu. 2004 Jan;22(1):30-2.

Abstract

A reversed-phase high performance liquid chromatographic method (HPLC) was established for determination of isothiocyanates in human urine, which used the reaction of propyl isothiocyanate with 1,2-benzenedithiol as reference instead of the synthesis of 1,3-benzodithiole-2-thione. The linear regression of the standard curve was determined to be y = 0.418 2 x + 2.821 (r2 = 0.999 3), that was well matched with the regression of methyl isothiocyanate, y = 0.412 2x + 2.442 3(r2 = 0.996 6). The detection limit (at approximately S/N = 2.5) was 0.08 micromol/L. The mean relative standard deviation (RSD) (n = 21) for the intra-day reproducibility was (4.7 +/- 2.9)%. The mean RSD (n = 4) for inter-day reproducibility of three samples was (7.0 +/- 5.0)%. The recovery of four propyl isothiocyanate standards was (91.3 +/- 7.9)% (mean RSD 8.7%). The initial results obtained by this method may provide useful information regarding to the kinetics of isothiocyanates in dietary consumption and excretion of individuals.

摘要

建立了一种反相高效液相色谱法(HPLC)用于测定人尿中的异硫氰酸盐,该方法以异硫氰酸丙酯与1,2 - 苯二硫醇的反应为参照,而非合成1,3 - 苯并二硫杂环戊烯 - 2 - 硫酮。标准曲线的线性回归方程为y = 0.418 2x + 2.821(r2 = 0.999 3),与异硫氰酸甲酯的回归方程y = 0.412 2x + 2.442 3(r2 = 0.996 6)匹配良好。检测限(约S/N = 2.5时)为0.08 μmol/L。日内重复性的平均相对标准偏差(RSD)(n = 21)为(4.7 ± 2.9)%。三个样品日间重复性的平均RSD(n = 4)为(7.0 ± 5.0)%。四个异硫氰酸丙酯标准品的回收率为(91.3 ± 7.9)%(平均RSD 8.7%)。该方法获得的初步结果可能为个体饮食摄入和排泄中异硫氰酸盐的动力学提供有用信息。

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