RESUMO
OBJECTIVE: To establish methods for the test of chemical dyes and quantitative determination of dracorhodin perchlorate in Guanmaining tablets. METHODS: HPLC-UV-MS/MS was used for the test of chemical dyes in Guanmaining tablets, and the concentration of dracorhodin perchlorate was determined by HPLC. In the test of chemical dyes, Agilent Zorbax-SB C18 (4.6 mm × 250 mm, 5 μm) was used as stationary phase, the mixture of 0.02 mol · L-1 ammonium acetate and acetonitrile was used as mobile phase in gradient elution mode, and the UV-Vis detection wavelength was set at 520 nm. ESI+ was used as ion source, and the MS/MS spectra of the analytes were recorded to confirm the positive results. In the quantitative analysis of dracorhodin perchlorate, Phenomenex Luna C18(4.6 mm × 250 mm, 5 μm) was used as stationary phase, the mixture of acetonitrile and 0.05 mol · L-1 sodium dihydrogen phosphate solution (37:63) was used as mobile phase, and the detection wavelength was set at 440 nm. RESULTS: Among 56 batches of Guanmaining tablets, 7 batches showed positive results of sudan I, sudan IV, and/or 808 scarlet. A good linear relationship was obtained in the range of 0.408 0 - 816.6 μg · mL-1 for dracorhodin perchlorate, with the linear regression equation of y = 1.746 1 × 107ρ +2 419.9(r = 1.000 0); the average recovery was 98.37% (RSD = 1.2%, n =6). The content of dracorhodin perchlorate in Guanmaining tablets ranged from 0.01 to 0.25 mg · tablet-1. CONCLUSION: The method is simple, accurate and rapid, and can be used for the quality control of Guanmaining tablets.
RESUMO
AIM: To develop a method of the HPLC/UV/MS/MS fingerprints of Qingkailing Injection(Radix Isatidis,Fructus Gardeniae,Flos Lonicerae Japonicae,etc.) and provide a novel conception for its quality control. METHODS: Separation was performed on Phenomenex Luna C_(18) analytical column(250 mm?4.6 mm,5 ?m).The mobile phases consisted of water containing 0.1% formic acid and acetonitrile was used as gradient elute.The flow rate was 1 mL/min.An Electrospray Ion Trap mass spectrometer was utilized for qualitative analysis and both positive and negative secondary ion scan mode were applied. RESULTS: Perfect fingerprints with excellent separation and reproducibility were obtained and 13 compounds were identified.Especially three isomers,including Neochlorogenic acid,Chlorogenic acid and Isochlorogenic acid,were differentiated successfully. CONCLUSION: The method is suitable for establishing the HPLC/MS/MS fingerprints of Qingkailing Injection and hence could be used as an effective and credible pattern for analyzing traditional Chinese medicine as well as its quality control.Moreover,based on this approch,further traditional Chinese medicine research can be performed.