title: Improved liquid chromatography combined with pulsed electrochemical detection for the analysis of etimicin sulfate.
abstract: This paper describes an improved liquid chromatography method combined with pulsed electrochemical detection for the analysis of etimicin sulfate. In total, 22 impurities could be separated. A TSK-GEL C18 column (250 mm × 4.6 mm i.d., 5 μm) is used, and the mobile phase is composed of 40 mL of acetonitrile and 960 mL of an aqueous solution containing trifluoroacetic acid (15 mL/L), pentafluoropropionic acid (500 μL/L), 50% sodium hydroxide (8 mL/L) and sodium sulfate (1.5 g/L). The pH of the aqueous solution is adjusted to 3.5 with 0.8 M sodium hydroxide. The influence of the different chromatographic parameters on the separation was investigated. A quadruple potential-time waveform was applied to the electrodes of the detection cell. 0.8 M sodium hydroxide was added post column to raise the pH to at least 12 before detection. A central composite experimental design was used to describe the relationship between factors and response values and to establish factorial analysis. Compared to previously published investigations, this improved method shows higher sensitivity, better separation ability and robustness and has been incorporated by the Chinese Pharmacopoeia 2015 for analysis of etimicin sulfate. A number of commercial samples of etimicin sulfate were also analyzed using this method.
authors.affiliation: Jiangsu Institute for Food and Drug Control, Nanjing, China.|China Pharmaceutical University, Nanjing, China.
authors.forename: Yuning
authors.initials: Y
authors.lastname: Wu
authors.affiliation: Jiangsu Institute for Food and Drug Control, Nanjing, China.
authors.forename: Wei
authors.initials: W
authors.lastname: Zhao
authors.affiliation: Jiangsu Institute for Food and Drug Control, Nanjing, China.
authors.forename: Xiaoyue
authors.initials: X
authors.lastname: Zhu
authors.affiliation: China Pharmaceutical University, Nanjing, China.
authors.forename: Fang
authors.initials: F
authors.lastname: Wang
authors.affiliation: Jiangsu Institute for Food and Drug Control, Nanjing, China.
authors.forename: Mei
authors.initials: M
authors.lastname: Zhang
authors.affiliation: Jiangsu Institute for Food and Drug Control, Nanjing, China.
authors.forename: Xialei
authors.initials: X
authors.lastname: Fan
authors.affiliation: Jiangsu Institute for Food and Drug Control, Nanjing, China.
authors.forename: Yaozuo
authors.initials: Y
authors.lastname: Yuan
authors.affiliation: National Institute for Food and Drug Control, Beijing, China.
authors.forename: Changqin
authors.initials: C
authors.lastname: Hu
authors.affiliation: Department of Pharmaceutical Analysis, School of Pharmacy, China Medical University, Shenyang, China.
authors.forename: Xiaolan
authors.initials: X
authors.lastname: Deng
authors.affiliation: Department of Pharmaceutical & Pharmacological Sciences, Pharmaceutical Analysis, KU Leuven, University of Leuven, Belgium.
authors.forename: Erwin
authors.initials: E
authors.lastname: Adams
mesh_terms: D002236:Carbohydrate Conformation; D002853:Chromatography, Liquid; D055664:Electrochemical Techniques; D005839:Gentamicins / Q000032:analysis*
chemical_list: D005839:Gentamicins; C555708:etimicin sulfate
keywords: Etimicin sulfate; Liquid chromatography; Pulsed electrochemical detection; Quadruple waveform