ABSTRACT
The study developed a method for the determination of 14 components in Bazibushen capsule by UPLC-ESI-MS/MS. Waters ACQUITY BEH C18 column (50 mm×2.1 mm, 1.7 μm) was used and the column temperature was 40℃. A linear gradient elution of eluents A (acetonitrile) and B (0.1% acetic acid) was used for the separation. The source temperature was set at 150℃. The capillary voltage was set at 2.0 kV. The source offset voltage was kept at 50 V. The desolvation temperature was set at 500℃. The desolvation flow was 800 L·h-1. The cone flow was 150 L·h-1. The nebuliser pressure was 7.0 Bar. Multiple reaction monitoring mode (MRM) is adopted. All of the 14 components showed good linearity (r2 > 0.999 1) in the test ranges. The LOQs for the compounds ranged from 0.11-4.52 ng·mL-1, respectively. The RSDs were 0.8%-2.1%. The overall recoveries were between 97.89% and 101.9% for all compounds. The method is simple, rapid, accurate and highly reproducible, and may be used in the determination of 14 components in Bazibushen capsule.
ABSTRACT
A GC-MS-SIM method was developed for the simultaneous determination of the 7 coumarins in common cnidium fruit. The 7 bioactive constituents were separated on DB-1 capillary column (30 m×0.25 mm, 0.25 μm) using temperature programming. The interface temperature was set at 280℃; Ion source temperature:250℃; Quadrupole temperature:150℃; EI mode:70 eV; The mass spectrometer detector was in SIM mode; Scan range:50-350 amu. All the 7 marker substances showed good linearity (r2>0.9986) in the test ranges. The LODs and LOQs for the compounds ranged from 1.06 to 10.11 ng ·mL-1 and from 3.21 to 29.88 ng·mL-1, respectively. The overall intra-day (n=6) and inter-day (n=3) RSDs were 0.7%-2.5% and 1.2%-3.3%, respectively. The overall recoveries were between 92.38% and 100.50% for all compounds. This method was simple, rapid, sensitive, with good specificity, and it can provide a reference for the quality control of common cnidium fruit.
ABSTRACT
This paper reports the establishment of a method for rapid identification 15 effective components of anti common cold medicine (paracetamol, aminophenazone, pseudoephedrine hydrochloride, methylephedrine hydrochloride, caffeine, amantadine hydrochloride, phenazone, guaifenesin, chlorphenamine maleate, dextromethorphen hydrobromide, diphenhydramine hydrochloride, promethazine hydrochloride, propyphenazone, benorilate and diclofenac sodium) with MRM by LC-MS/MS. The samples were extracted by methanol and were separated from a Altantis T3 column within 15 min with a gradient of acetonitrile-ammonium acetate (containing 0.25% glacial acetic acid), a tandem quadrupole mass spectrometer equipped with electrospray ionization source (ESI) was used in positive ion mode, and multiple reaction monitoring (MRM) was performed for qualitative analysis of these compounds. The minimum detectable quantity were 0.33-2.5 microg x kg(-1) of the 15 compounds. The method is simple, accurate and with good reproducibility for rapid identification many components in the same chromatographic condition, and provides a reference for qualitative analysis illegally added chemicals in anti common cold medicine.
Subject(s)
Acetaminophen , Acetanilides , Amantadine , Aminopyrine , Anti-Inflammatory Agents, Non-Steroidal , Antipyretics , Antipyrine , Caffeine , Chlorpheniramine , Chromatography, Liquid , Diclofenac , Diphenhydramine , Drug Contamination , Drug Stability , Ephedrine , Guaifenesin , Promethazine , Pseudoephedrine , Reproducibility of Results , Salicylates , Spectrometry, Mass, Electrospray Ionization , Tandem Mass SpectrometryABSTRACT
Objective: To establish a HPLC method to determinate the content of rocuronium bromide. Methods: NH2-bonding silica gel was used as the stationary phase. The mobile phase consisted of 0.04 mol/L tetramethyl ammonium hydroxide (pH adjusted to 7.4 by phosphoric acid) and acetonitrile (10:90). The column temperature was 35°C. The detection wavelength was 207 nm. Results: The relation between concentration and peak area was linear in the range of 0.1251-2.0065 mg/ml with r2 of 0.9999. The average recovery rate was 99.9% with RSD of 0.1%. Conclusion: This method is exclusive, sensitive and is reliable for the determination of rocuronium bromide.