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首页> 外文期刊>RSC Advances >Utilization of 7-chloro-4-nitrobenzo-2-oxa-1,3-diazole (NBD-Cl) for spectrochemical determination of l-ornithine: a multivariate optimization-assisted approach
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Utilization of 7-chloro-4-nitrobenzo-2-oxa-1,3-diazole (NBD-Cl) for spectrochemical determination of l-ornithine: a multivariate optimization-assisted approach

机译：利用7-氯-4-硝基苯乙烯-2-氧气-1,3-二唑（NBD-CL）的L-鸟氨酸的光谱测定：多变量优化辅助方法

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摘要

A simple and highly sensitive univariate calibration strategy based on ultraviolet-visible (UV-Vis) absorption spectroscopy and assisted by multivariate screening and optimization was utilized for the determination of l-ornithine (l-ORN) as such and in the alimentary supplements. l-ORN, an OTC marketed amino acid, is widely used for bodybuilding and might be abused by athletes. A nucleophilic substitution reaction using 7-chloro-4-nitrobenzo-2-oxa-1,3-diazole (NBD-Cl) was the basis of the current investigation. Plackett-Burman design (PBD) and a response surface optimizer as screening and fine-tuning strategies, respectively, were instigated. Four numerical variables, reaction time (RT), temperature (Temp), pH and reagent volume (RV), and one categorical variable, the diluting solvent (DS), were considered. Absorbance of the yellow-colored adduct at 469 nm was the response studied. Pareto analysis, along with analysis of variance (ANOVA) were used to ascertain the significant variables (screening phase) and their domains (optimization phase). Response transformation and stepwise analysis were employed when necessary. Probability, cube and individual value plots were used to get an insight into the statistical impact of the variables tested. Multiple responses' optimization was performed using Derringer's function. Calibration curves were linear in the range of 5-50 mu g mL(-1). Job's technique of continuous variation showed that the stoichiometric ratio is 2 : 1 (NBD-Cl : l-ORN). The proposed technique was successfully applied to the dietary supplements of l-ORN, inferring no interference from adjuvants and excipients. Analytical performance of this technique was validated conforming to the ICH standards.
机译：基于紫外线可见（UV-VIS）吸收光谱和通过多变量筛选和优化辅助的简单敏感的单变量校准策略用于测定L-鸟氨酸（L-ORN），如在消化物中。 L-ORN是一个OTC市场氨基酸，广泛用于健美，可能被运动员滥用。使用7-氯-4-硝基苯-2- OXA-1,3-二唑（NBD-CL）的亲核取代反应是当前研究的基础。 Plackett-Burman设计（PBD）和响应表面优化分别作为筛选和微调策略分别溶解。考虑了四种数值变量，反应时间（RT），温度（温度），pH和试剂体积（RV），以及一种分类变量，稀释溶剂（DS）。在469nm处的黄色加合物的吸光度是研究的响应。帕累托分析以及对方差分析（ANOVA）来确定显着的变量（筛选阶段）及其域（优化阶段）。必要时采用响应变换和逐步分析。概率，立方体和单独的价值地块用于了解所测试变量的统计影响。使用Derrier的功能进行多次响应优化。校准曲线在5-50μgmm（-1）的范围内是线性的。作业的连续变化技术表明，化学计量比为2：1（NBD-CL：L-ORN）。该提出的技术成功地应用于L-ORN的膳食补充剂，不推断不受辅助剂和赋形剂的干扰。这种技术的分析性能符合ICH标准。

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  • 来源
    《RSC Advances》 |2019年第38期|共10页
  • 作者

    Aly Hend; El-Shafie Ahmed S.; El-Azazy Marwa;

  • 作者单位

    Qatar Univ Coll Arts &

    Sci Dept Chem &

    Earth Sci Doha 2713 Qatar;

    Qatar Univ Coll Arts &

    Sci Dept Chem &

    Earth Sci Doha 2713 Qatar;

    Qatar Univ Coll Arts &

    Sci Dept Chem &

    Earth Sci Doha 2713 Qatar;

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  • 正文语种 eng
  • 中图分类 化学;
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