Abdelwahab Nada S, Fared Nehal F, Elagawany Mohamed, Abdelmomen Esraa H
Beni-Suef University, Faculty of Pharmacy, Pharmaceutical Analytical Chemistry, Beni-Suef, Egypt.
Damanhour University, Faculty of Pharmacy, Pharmaceutical Chemistry, Damanhour, Egypt.
J AOAC Int. 2017 Sep 1;100(5):1392-1399. doi: 10.5740/jaoacint.16-0322. Epub 2017 Feb 21.
Stability-indicating spectrophotometric, TLC-densitometric, and ultra-performance LC (UPLC) methods were developed for the determination of mepivacaine HCl (MEP) in the presence of its toxic impurity, 2,6-dimethylanaline (DMA). Different spectrophotometric methods were developed for the determination of MEP and DMA. In a dual-wavelength method combined with direct spectrophotometric measurement, the absorbance difference between 221.4 and 240 nm was used for MEP measurements, whereas the absorbance at 283 nm was used for measuring DMA in the binary mixture. In the second-derivative method, amplitudes at 272.2 and 232.6 nm were recorded and used for the determination of MEP and DMA, respectively. The developed TLC-densitometric method depended on chromatographic separation using silica gel 60 F254 TLC plates as a stationary phase and methanol-water-acetic acid (9 + 1 + 0.1, v/v/v) as a developing system, with UV scanning at 230 nm. The developed UPLC method depended on separation using a C18 column (250 × 4.6 mm id, 5 μm particle size) as a stationary phase and acetonitrile-water (40 + 60, v/v; pH 4 with phosphoric acid) as a mobile phase at a flow rate of 0.4 mL/min, with UV detection at 215 nm. The chromatographic run time was approximately 1 min. The proposed methods were validated with respect to International Conference on Harmonization guidelines regarding precision, accuracy, ruggedness, robustness, and specificity.
开发了稳定性指示分光光度法、薄层色谱-密度测定法和超高效液相色谱（UPLC）法，用于在其有毒杂质2,6-二甲基苯胺（DMA）存在的情况下测定盐酸甲哌卡因（MEP）。开发了不同的分光光度法用于测定MEP和DMA。在结合直接分光光度测量的双波长法中，221.4和240 nm之间的吸光度差值用于MEP测量，而二元混合物中283 nm处的吸光度用于测量DMA。在二阶导数法中，记录272.2和232.6 nm处的振幅并分别用于测定MEP和DMA。所开发的薄层色谱-密度测定法依赖于使用硅胶60 F254 TLC板作为固定相，甲醇-水-乙酸（9 + 1 + 0.1，v/v/v）作为展开系统进行色谱分离，并在230 nm处进行紫外扫描。所开发的UPLC法依赖于使用C18柱（250×4.6 mm内径，5μm粒径）作为固定相，乙腈-水（40 + 60，v/v；用磷酸调至pH 4）作为流动相，流速为0.4 mL/min，在215 nm处进行紫外检测。色谱运行时间约为1分钟。所提出的方法根据国际协调会议关于精密度、准确度、耐用性、稳健性和特异性的指导原则进行了验证。
