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用三氟乙酸测定亚硒酸甘油酯中硒(IV)的特定分光光度法。

Specific spectrophotometric method with trifluoroacetic acid for the determination of selenium(IV) in selenitetriglycerides.

作者信息

Suchocki P, Jakoniuk D, Fitak B A

机构信息

Department of Drugs Analysis, Warsaw Medical University, 1 Banacha Str., 02-097 Warsaw, Poland.

出版信息

J Pharm Biomed Anal. 2003 Aug 8;32(4-5):1029-36. doi: 10.1016/s0731-7085(03)00205-x.

Abstract

The role of selenium as an antioxidant and anticancer agent is very well documented in the literature. Selenium compound showing the highest activity as a free radicals scavenger and as an anticancer agent should contain selenium at +4 oxidation level. The synthesis of selenitetriglycerides (named selol) was carried out in the Department of Drug Analysis at Warsaw Medical University (Polish Patent 1999). Selenitetriglycerides showed a dimeric structure. In a single dose toxicity studies performed in rats, LD50 was 100 mg Se kg(-1) after oral administration of selol. The subcutaneous and intraperitoneal administration of selol showed extremely low toxicity. The aim of this work was to develop a new specific method for the determination of Se(IV) in selol. We stated that selenitetriglycerides react quantitatively with trifluoroacetic acid (TFA) in dichloromethane giving a red-coloured conjugate. However, recorded spectrum showed the maximum absorption in the wavelength 380 nm. The optimal conditions of the reaction were established, namely temperature 35 degrees C and reaction time 35 min. The reaction was proved to be specific because neither selenites nor other selol constituents react with TFA. The constructed calibration curve obeyed the Lambert-Beer law in the range of 0.1-7.4 mg ml(-1). Molar absorption coefficient is epsilon =9.46 x 10(3) l mol(-1) cm(-1) and epsilon =2.36 x 10(5) l mol(-1) cm(-1) calculated for selenium and selenitetriglyceride dimer (m.w. 1972.72), respectively. Obtained results for selenium determination were confirmed by AAS method. The developed method showed specificity and high sensitivity.

摘要

硒作为抗氧化剂和抗癌剂的作用在文献中有充分记载。作为自由基清除剂和抗癌剂表现出最高活性的硒化合物应含有氧化态为 +4 的硒。亚硒酸甘油三酯(称为硒醇)的合成是在华沙医科大学药物分析系进行的(波兰专利 1999)。亚硒酸甘油三酯呈现二聚体结构。在对大鼠进行的单剂量毒性研究中,口服硒醇后 LD50 为 100 mg Se kg⁻¹。皮下和腹腔注射硒醇显示出极低的毒性。这项工作的目的是开发一种测定硒醇中 Se(IV) 的新的特定方法。我们指出,亚硒酸甘油三酯在二氯甲烷中与三氟乙酸(TFA)定量反应生成红色共轭物。然而,记录的光谱显示在波长 380 nm 处有最大吸收。确定了反应的最佳条件,即温度 35℃,反应时间 35 分钟。事实证明该反应具有特异性,因为亚硒酸盐和其他硒醇成分均不与 TFA 反应。构建的校准曲线在 0.1 - 7.4 mg ml⁻¹ 范围内符合朗伯 - 比尔定律。对于硒和亚硒酸甘油三酯二聚体(分子量 1972.72)计算得到的摩尔吸收系数分别为 ε = 9.46×10³ l mol⁻¹ cm⁻¹ 和 ε = 2.36×10⁵ l mol⁻¹ cm⁻¹。通过原子吸收光谱法(AAS)对获得的硒测定结果进行了确认。所开发的方法具有特异性和高灵敏度。

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