Chemicalcharacterization of Jinming Tablet by HPLC-DAD/ELSD-ESI-TOF/MS and Study on the Multi-Index Quantitative Fingerprint / 中国药学杂志

OBJECTIVE: To analyze and identify the compositions using HPLC-DAD/ELSD-ESI-TOF/MS for establishing the multi index quantatitive HPLC fingerprint of the Jinming Tablet, in order to providing scientific basis for its quality control. METHODS: The Agilent SB C18 column (4.6 mm×250 mm, 5 μm) was used with a mobile phase of acetonitrile-0.2% acetic acid in gradient elution, the flow rate was 0.8 mL•min-1, the sample voume was 30 μL, the column temperature was maintaine at 25 ℃, the detection wavelength was set at 280 nm. ESI-TOF/MS positive and negative ion mode scanning was used to qualitatively analyze the components in methanol water extract from Jinming Tablet. RESULTS: Twenty compounds in Jinming Tablet extract could be primarily identified by HPLC-DAD on-line detection, in which five compounds were determined; based on the analysis of multiple batches of samples, the multi index chromatographic fingerprint was established, meanwhile combined with similarity analysis to achieve the quality evaluation of Jinming Tablet. CONCLUSION: The HPLC-DAD/ELSD fingerprint film analysis method for Jinming Tablet is established, which could provide reference for the quality control of the material basis of other compound.

Multi-components determination and fringerprints analysis by HPLC in Chaenomeles thibetica / 中草药

Objective To establish a HSDE-HPLC-DAD-ESI-TOF/MS method for the rapid identification of chemical ingredients for Chaenomeles thibetica, and establish the multi-component quantitative fingerprint to evaluate its quality. Methods The separation was developed via an Agilent Zorbax SB-C18 column (250 mm × 4.6 mm, 5.0 μm) with a gradient elution at a temperature of 25 ℃, the acetonitrile was used as the mobile phase A and 0.5% glacial acetic acid and 10 mM ammonium acetate solution was used as the mobile phase B with a flow rate of 0.8 mL/min, and the detection wavelength was 280 nm. ESI-TOF/MS was used for the identification of chemical ingredients in C. thibetica. The fingerprint of C. thibetica was established based on the quantitative detection of multi-components. Results The HPLC fingerprint of C. thibetica has 30 common peaks, nine ingredients (chlorogenic acid, vanillic acid, caffeic acid, veratric acid, rutin, quercitrin, hyperin, oleanolic acid, and uosolic acid) of C. thibetica were identified, and the contents of them were determined. Similarity analysis shows that the similarity of 10 batches of C. thibetica is relatively close, while the similarity between C. thibetica and other varieties' is quite different. Conclusion HSDE-HPLC-DAD-ESI-TOF/MS method can be used for the rapid extraction and analysis of C. thibetica fresh samples. On this basis, the fingerprint analysis combined with similarity analysis can be used for quality evaluation of C. thibetica.

Quick Separation and Identification of 24 Chemical Constituents in Radix Astragali by HPLC-ESI-TOF/MS / 中国药师

Objective:To analyze the chemical constituents in Radix astragali by high-performance-liquid chromatography-time of flight mass spectrometry(HPLC-TOF/MS). Methods:An Agilent poroshell 120 SB-C18 column(100 mm × 3 mm,2. 7 μm)was adopt-ed. The mobile phase was composed of acetonitrile-0. 1% formic acid with nonlinear gradient elution. The flow rate was 0. 4 ml· min-1 . The UV detection wavelength was set at 254nm, the column temperature was 25℃ and the injection volume was 10μl. Electron spray ionization and positive mode was adopted, the flow and temperature of the carrier gas( N2 ) was 10 L·min-1 and 350℃, respec-tively. The capillary voltage was 4 kV, the bombardment voltage was 165 V, the spectra were recorded within the range of m/z 100~1 100. Results:A total of 24 chemical constituents were identified from Radix astragali by HPLC-TOF/MS simultaneously. Conclu-sion:An efficient and fast HPLC-TOF/MS approach has been established for studying the chemical constituents in Radix astragali, which lays the foundation for the study on pharmacodynamic material basis and quality control of Radix astragali.

Screening and identification of multiple components in Tanreqing injection using RP-HPLC combined with DAD and ESI-TOF/MS / 中国天然药物

A liquid chromatography coupled with diode array detector (DAD) and electrospray ionization time-of-flight mass spectrometry (ESI-TOF/MS) method was developed for the screening and identification of the multiple components in Tanreqing injection, a well-known Chinese medicine injection in China. By combining the DAD spectrum and the accurate mass measurement of ESI-TOF/MS, twelve components in Tanreqing injection were identified. This study contributes to clarifying the nature of Tanreqing injection, and provides an effective and reliable process for the comprehensive and systematic characterization of complex traditional Chinese medicine preparations.

Identification of compounds in aqueous extract from aerial parts of Lycopus lucidus by HPLC-ESI-TOF-MS/MS / 中草药

Objective: To identify the main active compounds in the aqueous extract from the aerial parts of Lycopus lucidus by high performance liquid chromatography (HPLC)-electrospray (ESI)-time of flight tandem mass spectrometry (TOF-MS/MS). Methods: The aqueous extract from the aerial parts of L. lucidus was prepared using ultrasonic method; Chromatographic separation of the main active compounds was performed on a TC-C18 (250 mm × 4.6 mm, 5 μm) reverse phase column through gradient elution; All the compounds eluted from the column were detected under both positive and negative ionization modes. Each chromatographic peak was analyzed by quadrupole tandem mass spectrometry coupled with TOF. Results: Twenty two compounds were identified through the analysis of tandem mass spectrum and the information from reference substances, including amino acids, phenolic acids, terpenoids, flavonoids and flavonoid glycosides, sterols, and fatty acid. Conclusion: HPLC-ESI-TOF-MS/MS is capable of analyzing the main compounds in the aerial parts of L. lucidus using retention time, ultraviolet spectrum, current molecular weight, formula, and fragmenting information of daughter ions. It will probably become a reliable alternative for the rapid analyzing substantial foundation of Chinese materia medica.

HPLC Fingerprint and LC-TOF-MS Analysis on Extract from Roots of Gentiana macrophylla / 中草药·英文版

Objective Establishing a fingerprint method to identify the characteristic chemicals in the roots of Gentiana macrophylla and evaluate their quality.Methods RP-HPLC was developed for fingerprint analysis and determination of four ingredients in G macrophylla roots from different sources.LC-ESI-TOF-MS was employed to identify the chromatographic peaks of the fingerprint.Results Five common peaks were identified by comparing their retention time with reference secoiridoid glucosides.Eight major peaks in chromatographic fingerprint were analyzed by on-line LC-ESI-TOF-MS.Four secoiridoid glucosides were identified based on their MS data.Conclusion The method is specific and could be served for the quality identification and comprehensive evaluation of G macrophylla.

Analysis of coumarins in extract of Cnidium monnieri by ultra-performance liquid chromatographic coupled to electrospray ionization time of flight mass/mass spectrometry / 中成药

AIM: To set up a rapid analysis and characterization method for coumarins in extract of Cnidium monnieri. METHODS: The sample was analyzed by ultra-performance liquid chromatography with a reversed phase C_(18) column using a binary eluent of acetonitrile and water(with 0.1% formic acid) under gradient conditions.The ~+ ions of coumarins in Cnidium monnieri extract were observed by positive ion electrospray time of flight mass spectrometry (ESI-TOF-MS) online detection,and the fragmentation behavior obtained by ESI-TOF-MS/MS,then coumarins was identified through accurate molecular weight and molecular formula and fragmentation information combined with literature review. RESULTS: All components could be separated rapidly within 10 min,and five coumarins-xanthotoxol,bergapten,xanthotoxin,imperatorin and osthol could be primary identified in Cnidium monnieri extract. CONCLUSION: This method is effective for identification of coumarins in extract of Cnidium monnieri.