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@#The aim of the study was to develop a simple, rapid and accurate LC-MS/MS method for the determination of digoxin.Digoxin-d3 was taken as the internal standard (IS), and sample preparation was achieved by liquid-liquid extraction.Chromatographic separation was performed on a Kinetex C18 column (2.1 mm × 50 mm, 2.6 μm; Phenomenex) using an isocratic elution with merely 2 min for each sample.The mobile phase consisted of water and acetonitrile solutions, both containing 1 mmol/L ammonium acetate and 1 mmol/L formic acid (55∶45).The detection was conducted on a TripleQuadTM 4500MD mass spectrometer coupled with electrospray ionization interface under positive-ion multiple reaction monitoring mode.The transitions were m/z 798.5 → 651.3 and m/z 801.6 → 654.4 for digoxin and digoxin-d3, respectively.Results showed that the method was linear over the range of 0.100-20.0 ng/mL.The selectivity, accuracy and precision, recovery and stability of the method were all within the acceptable limits with no matrix effect.This method was successfully applied to a girl treated with digoxin with substantial improvement of therapeutic effect and elimination of toxic reaction, so it can provide valuable fuidance and reference for individualized medication in clinical practice.
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Aim: To develop and compare the ultra-performance liquid chromatography( UPLC) and HPLC methods for the determination of dihydroflavonoids in Smilacis glabrae Rhizoma, and establish the quality evaluation system of the above-mentioned crude drug. Methods: Four dihydroflavonoids in the crude drugs collected from 15 localities were determined using the UPLC and HPLC methods, respectively. The resolution, sensitivity, precision, accuracy and the content determination results of the four compounds were compared between the two methods. Results: The UPLC method was more fast and sensitive than the HPLC method with no significant differences among the linearity range, precision, accuracy and the content determination results between the two methods. Conclusion: The developed HPLC method was proved practicable and reliable for the quality control of Smilacis glabrae Rhizoma. The UPLC method was provided to be a more sensitive, fast and solvent-saving method compared to HPLC and can be applied in the quality evaluation of Chinese medicines.
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OBJECTIVE:To establish a rapid determination method for gentaminin active components.METHODS:Scan-TLC procedure was applied.A mixture of methanol-chloroform-28%ammonium hydroxide(1∶1∶1)was taken as developing reagent and ninhydrin in a mixtrue solvent as reveal reagent.The detecting wavelength was500nm.RESULTS:The amounts of three components in gentamincin per spot were linear in the range of2?g～12?g(r 1 =0.9993、r 2 =0.9996、r 1a =0.9991).CONCLUSION:This scan-TLC technique is recommendable for determination of gentamincin components.