ABSTRACT
This paper first briefly introduces the basic information of aminoglycosides for pharmaceutical use such as origin, classification, chemical structures, diversity of composition and the research originators, etc. Then it reviews the development process of the technologies for the analysis of components of aminoglycosides, discusses the advantages and disadvantages of current methodologies and explains the advantage of liquid chromatography coupled with pulsed amperometric detection method for analysis of the components of aminoglycosides. At last, it introduces some new analysis technologies and ideas and forecasts the direction of future development.
ABSTRACT
OBJECTIVE: To establish an LC/MSn method for identification of the related substances in etimicn sulfate detected under the chromatographic condition described in Chinese Pharmacopoeia 2010. METHODS: The HPLC separation was carried out on a Welch Ultimate LP-C18 column (4.6 mm × 300 mm, 5 μm) with mobile phase consisting of 0.2 mol · L-1 trifluoroacetic acid (containing 0.1% propionic acid ) -methanol (84: 16) at a flow rate of 1.0 mL · min-1. Thirty percent of the eluent was detected by ion trap mass spectrometry, and the parent ions and the corresponding product spectra of all the related substances in etimicin sulfate were determined and elucidated. RESULTS: Addition of 0.1% propionic acid into the mobile phase significantly enhanced the sensitivity of MS detector without altering the chromatographic behavior such as retention time and elution order of the related substances. Twenty-eight related substances were separated and detected by the LC/MSn method in a typical sample. Nine of them were identified with the help of corresponding impurity reference substances and 14 of them were elucidated by MS fragment information, while the other five were not identified due to limitated information. CONCLUSION: The established method can be applied to the identification of the related substances in etimicn sulfate detected under the chromatographic condition described in Chinese Pharmacopoeia 2010, which is helpful to the quality improvement and process optimization of etmicin sulfate.
ABSTRACT
To study the related substances in purified alliin, HPLC-MS/MS method carried out on a Phenomenex NH2 column was used for screen and identification of the related substances with full scan MS spectra determination of their [M + H] + ions and then the analyses of the retention time, product MS spectra and/or chemical reference standards. The full scan HPLC-MS chromatogram showed that there were seven major related substances in the purified alliin and their m/z of the [M + H] + ions with increasing retention were 116, 133, 147, 152, 175, 178 and 178, separately. And they were identified as proline, asparagine, glutamine, methiin, arginine, isoalliin and cycloalliin (both were isomers of alliin), respectively. The major related substances in purified alliin are amino acids, homologen and the isomers of alliin.
Subject(s)
Chromatography, High Pressure Liquid , Methods , Cysteine , Tandem Mass Spectrometry , MethodsABSTRACT
<p><b>AIM</b>To investigate whether tazobctam has crystallization water.</p><p><b>METHODS</b>In order to establish a method for water content determination in tazobctam, many methods including Karl Fischer titration, weight loss on drying, TGA, DSC and X-ray diffraction experiment of an orthorhombic form were studied.</p><p><b>RESULTS</b>The water content of the same batch tazobactam determined by different mthods was different.</p><p><b>CONCLUSION</b>The results showed that one mole tazobatam contains half mole water of crystallization and the strength of attraction between tazobatam molecule and water molecule is rather strong.</p>