Identification and Analysis of Chemical Components in Zhideke Granules by UPLC-Q-Orbitrap HRMS

[Objectives]To identify and analyze chemical components in Zhideke Granules by ultra performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry(UPLC-Q-Orbitrap HRMS).[Methods]Zhideke Granules were isolated on a Thermo Hypersil Gold C18 column(2.1 mm×100 mm,1.9μm).The mobile phase was 0.1%formic acid acetonitrile and 0.1%formic acid aqueous solution(containing 10 mmol ammonium acetate)with gradient elution.Chemical components in Zhideke Granules were rapidly isolated and identified by HRMS in the positive and negative ion mode with full scan data-dependent two stage threshold-triggered mass modes(Full MS/dd-MS2).[Results]The secondary fragment ion information of the target compound was selected and compared with the compound reported in the databases and related literatures for further confirmation.In total,30 chemical compounds were identified,including 12 flavonoids and glycosides,9 organic acids,3 nitrogen-containing compounds,and 6 other components.[Conclusions]In this study,the UPLC-Q-Orbitrap HRMS was used for the first time to analyze the chemical components in Zhideke Granules.It is intended to provide a reference for the quality evaluation and further study of pharmacodynamic materials of Zhideke Granules.

Microbial Limit Test of Zhideke Granules

[Objectives]To test the microbial limit of Zhideke granules.[Methods]According to the relevant regulations on the testing of granules in Chinese Pharmacopoeia in 2015,the applicability of the methods for counting the total number of aerobic bacteria,molds and yeasts and objectionable organisms in Zhideke granules was studied.[Results]The total number of aerobic bacteria in Zhideke granules was determined by dilution plate method(1∶20,1 mL per dish),the total number of molds and yeasts was determined by conventional plate method(1∶10,1 mL per dish),and E.coli was detected by conventional method of TTB(1∶10 test solution,10-100 mL TSB).[Conclusions]The method was suitable for the microbial limit test of Zhideke granules.