Li Wei, Wang Jun, Yan Zheng-Yu
Department of Analytical Chemistry, China Pharmaceutical University, 24 Tongjia Lane, Nanjing 210009, China; Key Laboratory of Drug Quality Control and Pharmacovigilance, Ministry of Education, 4 Tongjia Lane, Nanjing 210009, China; Department of Antibiotics, Anhui Institute for Food and Drug Control, Hefei 230051, China.
School of Medical Engineering, Hefei University of Technology, Hefei 230009, China.
J Pharm Biomed Anal. 2015 Oct 10;114:341-7. doi: 10.1016/j.jpba.2015.06.012. Epub 2015 Jun 15.
A novel simple, fast and efficient supercritical fluid chromatography (SFC) method was developed and compared with RPLC method for the separation and determination of impurities in rifampicin. The separation was performed using a packed diol column and a mobile phase B (modifier) consisting of methanol with 0.1% ammonium formate (w/v) and 2% water (v/v). Overall satisfactory resolutions and peak shapes for rifampicin quinone (RQ), rifampicin (RF), rifamycin SV (RSV), rifampicin N-oxide (RNO) and 3-formylrifamycinSV (3-FR) were obtained by optimization of the chromatography system. With gradient elution of mobile phase, all of the impurities and the active were separated within 4 min. Taking full advantage of features of SFC (such as particular selectivity, non-sloping baseline in gradient elution, and without injection solvent effects), the method was successfully used for determination of impurities in rifampicin, with more impurity peaks detected, better resolution achieved and much less analysis time needed compared with conventional reversed-phase liquid chromatography (RPLC) methods.
开发了一种新型的简单、快速且高效的超临界流体色谱（SFC）方法，并将其与反相液相色谱（RPLC）方法进行比较，用于分离和测定利福平中的杂质。使用填充二醇柱和由含0.1%甲酸铵（w/v）和2%水（v/v）的甲醇组成的流动相B（改性剂）进行分离。通过优化色谱系统，获得了利福平醌（RQ）、利福平（RF）、利福霉素SV（RSV）、利福平N-氧化物（RNO）和3-甲酰基利福霉素SV（3-FR）总体令人满意的分离度和峰形。通过流动相梯度洗脱，所有杂质和活性成分在4分钟内分离。充分利用SFC的特点（如独特的选择性、梯度洗脱时无基线倾斜以及无进样溶剂效应），该方法成功用于利福平中杂质的测定，与传统反相液相色谱（RPLC）方法相比，检测到更多杂质峰，实现了更好的分离度，且所需分析时间更短。
