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A sensitive chromatographic determination of hydrazines by naphthalene-2,3-dialdehyde derivatization

机译:萘-2,3-二醛衍生化反应灵敏色谱法测定肼

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A new high-performance liquid chromatography (HPLC) method for the sensitive simultaneous determination of hydrazine (Hy), monomethylhydrazine (MMH) and 1,1-dimethylhydrazine (UDMH) based upon the derivatization of hydrazines with naphthalene-2,3-dialdehyde and the separation of the derivatives on Zorbax Eclipse AAA column in a single chromatographic run under acidic conditions (pH 2.4) was developed. Hydrazine and monomethylhydrazine derivatives were found to be strongly fluorescent at λ_(ex) = 273 nm, λ_(em) = 500 nm. It was shown that UDMH derivative can be detected as non-fluorescent hydrazone at 290 nm by UV-detection. Limits of detection were 0.05 μg•L~(-1) for Hy and MMH, and 1 μg • L~(-1) for UDMH for the injection volume of 100 μL. The method was validated for water sample analysis. It proved to be selective, accurate and precise with the supplementary advantage of the simple and rapid sample preparation.
机译:基于肼与萘-2,3-二醛和萘的衍生化反应的灵敏的同时测定肼(Hy),一甲基肼(MMH)和1,1-二甲基肼(UDMH)的高效液相色谱(HPLC)新方法开发了在酸性条件下(pH 2.4)进行单次色谱分离的Zorbax Eclipse AAA色谱柱上的衍生物分离方法。发现肼和一甲基肼衍生物在λ_(ex)= 273 nm,λ_(em)= 500 nm时具有强荧光。结果表明,通过紫外检测,UDMH衍生物可以在290 nm处检测为非荧光。对于进样量为100μL,Hy和MMH的检出限为0.05μg•L〜(-1),对于UDMH为1μg•L〜(-1)。该方法已经过水样分析的验证。事实证明,它具有选择性,准确和精确的特点,并具有简单快速的样品制备的补充优势。

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