ABSTRACT
A global quality control method based on high performance liquid chromatography (HPLC) coupled with diode array detection (DAD), single quadrupole mass spectrometry (MS) and time-of-flight mass spectrometry (TOFMS) was developed for simultaneous determination of seven major components (mangiferin, neomangiferin, timosaponin E1, timosaponin E, timosaponin BII, timosaponin BIII, and timosaponin A III) and identification of most components in extracts of Rhizoma Anemarrhenae (RA). HPLC analysis was performed on an Agilent SB-C18 column (4.6 mm X 150 mm, 5 μm) by gradient elution using acetonitrile and water-acetic acid(100:0.05, v/v) as the mobile phase. Seven major components in RA were successfully separated. This quantitative method was fully validated in respect of the following performance criteria, linearity, precision, repeatability, stability, accuracy, limits of detection (LOD) and quantification (LOQ). A formula database of known compounds in RA was established, against which, most of the reported components in this herbal extract were identified effectively based on the extract masses acquired by TOFMS. This qualitative and quantitative method was successfully used to analyze the components in 10 batches of RA samples collected from different regions in China. This global quality control method, which consisted of HPLC-DAD-MS assay of seven major components and unambiguous identification of nineteen components, is suitable for routine quantification and comprehensive quality control of RA.
ABSTRACT
Objective To rapidly separate and identify the chemical components in traditional Chinese herbal medicine of Oldenlandia diffusa and its injection preparations by high performance liquid chromatography-time of flight mass spectrometry (HPLC-TOFMS). Methods An Agilent Zorbax XDB-Q18 column (250 mm×4. 6 mm, 5 μm) was used for separation and identification of chemical components in Oldenlandia diffusa, with a mobile phase of 0. 3% acetic acid (A) and methanol (B) in gradient elution, 0-30 min, 30%-90%B. The flow rate was set at 1. 0 ml/min and the injection volume was 10 μl. The time- of-flight mass spectrometer was equipped with an EIS ion source. The scanning mass range was between m/z 100-1 000. Results The traditional Chinese medicine of Oldenlandia diffusa and its injection preparation were on-line separated and characterized by HPLC-TOFMS, and 11 chemical compounds were identified in Oldenlandia diffusa, 6 compounds in market injection preparation, and 2 compounds in the injection prepared by ourselves. Conclusion Chromatographic demonstration of chemical compounds in Oldenlandia diffusa in one run provides a foundation for the further studying the metabolism and mechanism of Oldenlandia diffusa and its injection preparations.
ABSTRACT
A global quality control method based on high performance liquid chromatography (HPLC) coupled with diode array detection (DAD), single quadrupole mass spectrometry (MS) and time-of-flight mass spectrometry (TOFMS) was developed for simultaneous determination of seven major components (mangiferin, neomangiferin, timosaponin E1, timosaponin E, timosaponin BⅡ, timosaponin BⅢ, and timosaponin AⅢ) and identification of most components in extracts of Rhizoma Anemarrhenae (RA). HPLC analysis was performed on an Agilent SB-C18 column (4.6 mm×150 mm, 5 μm) by gradient elution using acetonitrile and water-acetic acid(100∶0.05, v/v) as the mobile phase. Seven major components in RA were successfully separated. This quantitative method was fully validated in respect of the following performance criteria: linearity, precision, repeatability, stability, accuracy, limits of detection (LOD) and quantification (LOQ). A formula database of known compounds in RA was established, against which, most of the reported components in this herbal extract were identified effectively based on the extract masses acquired by TOFMS. This qualitative and quantitative method was successfully used to analyze the components in 10 batches of RA samples collected from different regions in China. This global quality control method, which consisted of HPLC-DAD-MS assay of seven major components and unambiguous identification of nineteen components, is suitable for routine quantification and comprehensive quality control of RA.