Clavulanate potassium in the related substances in HPLC - ESI - MS analysis.docVIP

 PAGE \* MERGEFORMAT 8 Clavulanate potassium in the related substances in HPLC / ESI / MS analysis [Abstract] Objective examination and deduction of potassium clavulanate in the related substances. Methods HPLC / ESI / MS LC-MS technology, liquid chromatography conditions: column C18 (250mm * 4.6mm, 5μ m); column temperature 40 ℃ ; mobile phase A of 0.01mol / L ammonium acetate mobile phase B as mobile phase A and acetonitrile (1:1) mixture; flow rate 1ml/min; post-column diversion 1:1; Detection: UV230; linear gradient elution. MS conditions: Ion source: ESI; detection mode: positive and negative ions two kinds of forms; scan range: 50 ~ 800m / z; ionization voltage: 3.0kV; electrospray ionization interface, dry gas (N2) flow rate of 318L / h; ion source temperature 150 ℃ ; tapered bore voltage 30V. The results from the clavulanate potassium in the isolated and identified six kinds of related substances, of which 3 species and related substances listed in the European Pharmacopoeia the same. Conclusion clavulanate potassium in the production process to generate a variety of related substances, the method for the study and identification of related substances and clavulanate potassium sources, improve quality and safety of drugs provides the technical support. [Keywords:] clavulanate potassium; LC-MS technology; related substances ABSTRACT Objective To analyze the related substances in clavulanate potassium. Methods HPLC, electrospray ionzation and selective ion monitoring mass spectrum method were used; the HPLC condition: column C18 (250 mm * 4.6 mm, 5 μ m), temp: 40 ℃ , mobile phase : A) 0.01 mol / L ammonium acetic; B) mixture of mobile phase A and acetonitrile (1:1); flow rate: 1 ml / min; postcolumn split ratio: 1:1; detection: UV 230nm; elute by linear gradient . MS parameter: ion source: ESI (); 50 ~ 800 m / z; ionization voltage: 3.0 kV; dry gas (N2) flow rate: 318 L / h; temp: 150 ℃ ; emale cone voltage: 3.0 kV. Results Six related substances were