Determination of Glucocorticoids Illegally Added in Preparations of Medical Institutions by HPLC-ITMS
Objective:A high performance liquid chromatography-ion trap mass spectrometry(HPLC-ITMS)method was developed for the rapid screening of 15 kinds of glucocorticoids illegally-added in the preparations of medical institutions.Methods:The samples were pre-processed with acetonitrile by vortex extraction,and separated on Shiseido CAPCELL-PAK C18 column by gradient elution with 0.2%acetic acid aqueous solution-0.2%acetic acid acetonitrile solution as mobile phases,and detected by MS and MS2 after ionization with electrospray ionization source(ESI)in positive ion scanning mode.The column temperature was set to 25 ℃ with flow rate of 0.5 mL·min-1.Results:The chromatographic peaks of 15 compounds can be completely separated with the developed HPLC-ITMS condition.The detection limits of this method are 0.05~1.00 mg·kg-1.No glucocorticoid ingredients were detected in the 20 batches of medical insti-tution preparations.Conclusion:This method was specific,simple to operate,sensitive,and suitable for qualitative screening of 15 glu-cocorticoids illegally added to preparations of medical institutions.
Preparations in medical institutionsGlucocorticoidsIllegal additionHigh performance liquid chromatography ion trap mass spectrometry(HPLC-ITMS)