Analytical Chemistry Department, Faculty of Pharmacy, Cairo University, Giza, Egypt.
Chemistry Department, School of Pharmacy and Pharmaceutical Industries, Badr University in Cairo, Badr City, Egypt.
Chirality. 2019 Oct;31(10):835-844. doi: 10.1002/chir.23116. Epub 2019 Aug 1.
Chiral stationary phases are conveniently used for enantiomeric separation of drugs by liquid chromatography. Consumption of large volumes of hazardous solvents is considered as a common challenge for the sustainability of this technique. To this end, a columnar chromatography has been adopted using 50-mm-length stationary phases. The study comprised five Phenomenex Lux cellulose- and amylose-based columns for the separation of guaifenesin (GUA) enantiomers. In addition, an experimental design was used to optimize the gradient profile for the separation of racemic GUA and ambroxol HCl (AMB) binary mixture. The chromatographic method was achieved using Lux Cellulose-1 (50 × 4.6 mm) as a chiral stationary phase and ethanol/water as a mobile phase with linear gradient elution of 20% to 70% ethanol in 6 minutes at a flow rate of 1.0 mL min and UV detection at 270 nm. Linearity ranges were found to be 50 to 1000 μg mL and 15 to 450 μg mL for each GUA enantiomer and AMB, respectively. Environmental, health and safety tool was used to assess and compare greenness of the proposed and reported methods. Short column indeed reduces the environmental impact by decreasing waste by about 60% and utilizing only 1-mL ethanol in the mobile phase. The proposed method is a safer alternative for the simultaneous determination of drugs in their combined pharmaceutical formulation. The method has been validated and compared favorably with a reported one.
手性固定相在药物对映体拆分的液相色谱中应用广泛。大量使用危险溶剂是该技术可持续性的一个常见挑战。为此,采用了柱层析法,使用 50mm 长的固定相。该研究采用了五根 Phenomenex Lux 纤维素和直链淀粉基柱,用于分离愈创甘油醚(GUA)对映体。此外,还采用实验设计优化了用于分离外消旋 GUA 和盐酸氨溴索(AMB)二元混合物的梯度轮廓。采用 Lux Cellulose-1(50×4.6mm)作为手性固定相,乙醇/水作为流动相,以 1.0mL/min 的流速进行 6 分钟线性梯度洗脱,从 20%到 70%乙醇,在 270nm 处进行紫外检测,实现了色谱方法。每个 GUA 对映体和 AMB 的线性范围分别为 50 到 1000μg/mL 和 15 到 450μg/mL。采用环境、健康和安全工具评估和比较了所提出和报道方法的绿色度。短柱确实通过减少约 60%的废物和仅在流动相中使用 1 毫升乙醇来减少环境影响。该方法是同时测定其复方制剂中药物的更安全替代方法。该方法已得到验证,并与已报道的方法进行了比较。