Lozano-Olvera Carlos E, Lopez-Tellez Jorge, Ibarra Israel S, Miranda Jose M, Rodriguez Jose A
Area Academica de Quimica, Universidad Autonoma del Estado de Hidalgo, Pachuca, Hidalgo, Mexico.
Laboratorio de Higiene, Departamento de Quimica Analitica Nutricion y Bromatología, Inspeccion y Control de Alimentos, Universidad de Santiago de Compostela, Lugo, Spain.
Anal Bioanal Chem. 2025 Aug;417(20):4549-4555. doi: 10.1007/s00216-025-05947-4. Epub 2025 Jun 5.
A micellar electrokinetic chromatography (MEKC) methodology was optimized for the indirect determination of glycerol based on formaldehyde formation and the use of 3-methyl-2-benzothiazolinone hydrazone (MBTH) as a derivatizing agent. A Taguchi experimental design matrix L(3) was used to evaluate the critical variables and maximize the separation efficiency. Under optimum conditions of [SDS] 60.0 mM, [Na₂B₄O₇] 25.0 mM, and a pH value of 9.0, the methodology provides a linear interval range (0.18-0.91% w/w), a limit of detection (0.06% w/w), with satisfactory results in terms of intra-day and inter-day precision %RSD < 6.0% in all cases. The proposed methodology was applied to real biodiesel samples, and the results were compared with the official standard methodology in the determination of glycerol content (%w/w). The analysis of eight samples yielded results ranging from 0.12 to 0.20% w/w, and no differences were observed. The proposed methodology was applicable to quantifying glycerol at the concentration levels established by international norms.
基于甲醛形成以及使用 3 - 甲基 - 2 - 苯并噻唑啉酮腙（MBTH）作为衍生剂，对胶束电动色谱（MEKC）方法进行了优化，用于间接测定甘油。采用田口实验设计矩阵L(3)来评估关键变量并最大化分离效率。在[SDS] 60.0 mM、[Na₂B₄O₇] 25.0 mM以及pH值为9.0的最佳条件下，该方法提供了线性区间范围（0.18 - 0.91% w/w）、检测限（0.06% w/w），在所有情况下日内和日间精密度%RSD < 6.0%，结果令人满意。将所提出的方法应用于实际生物柴油样品，并将结果与官方标准方法在甘油含量（%w/w）测定方面进行比较。对八个样品的分析结果为0.12至0.20% w/w，未观察到差异。所提出的方法适用于按照国际规范确定的浓度水平对甘油进行定量。
