ABSTRACT
Evaporative light scattering detector(ELSD) and charged aerosol detector(CAD) methods were established in this study for the content determination of four kinds of sugars in Zhusheyong Yiqi Fumai(YQFM), and the factors affecting the accuracy of CAD methods were discussed. HPLC-ELSD chromatographic separation was performed on a Shodex Asahipak NH2 P-50 column with acetonitrile-water(75∶25)as the mobile phase, with a flow rate of 0.8 mL·min~(-1), drift tube temperature of 80 ℃. The analysis by HPLC-CAD was performed on the same column with acetonitrile-water as mobile phase for gradient elution, with a flow rate of 0.8 mL·min~(-1), a neb temperature of 45 ℃, and power function(PF) of 1.3. The samples of YQFM were detected by ELSD and CAD respectively. It was found that YQFM was composed of fructose, glucose, sucrose and maltose. The linear relationship of the two methods was good, and the recoveries, reproducibility and stability of these four kinds of sugars measured by the two methods satisfied the requirements of methodology. Both CAD and ELSD detectors were accurate and reliable in detecting saccharides components in YQFM. In addition, it was revealed in this study for the first time that the PF parameter of CAD had an important influence on the accuracy of sugar determination and acted as the key parameter of CAD method. It was also found that for CAD, a non-linear detector, there was no significant difference between the results of linear regression and logarithmic regression.
Subject(s)
Aerosols , Carbohydrates , Chromatography, High Pressure Liquid , Light , Reproducibility of Results , Scattering, Radiation , SugarsABSTRACT
In recent years, charged aerosol detector(CAD)has become a valuable tool for detecting substances with no ultraviolet absorption or with only end absorption. Its advantages inclucle broad linearity response range, high sensitivity and reproducibility, the signal response consistency independent of chemical structures, as well as the simply operable feature. This article briefly describes the working principle of CAD and introduces the application progress of the detector in the natural product and pharmaceutical detection as well as in the sugar, lipid, amino acid and surfactant analysis, so as to provide a reference for the liquid chromatographic analysis of non-volatile and semi-volatile compounds.
ABSTRACT
Objective To develop a method for the determination of five furostanol saponins(timosaponin N,timosaponin L, timosaponin BⅡ,25R-timosaponin BⅡ,and 25S-officinalisnin-Ⅰ)in rhizome and fibrous root of Anemarrhena asphodeloides Bge. by HPLC with the charged aerosol detector(CAD). Methods The analysis was performed on TechMate C18-ST-II(250 mm×4.6 mm,5μm)with acetonitrile:water(22:78,V/V),the flow rate of 1.0 ml/min and column temperature at 30℃. The Corona parameters were as follows:sampling rate 10 Hz,filter 5 s,and the nebulizer temperature 55℃. Results The approach showed good linearity for five saponins. The correlation coefficients(r2)for calibration curves varied from 0.9992 to 0.9998. The limits of detection(LOD)were 0.28,0.92,0.92,0.92 and 0.92 ng for five steroidal saponins,respectively. The limits of quantitation(LOQ)were found to be 0.92, 2.77,2.77,2.77 and 2.76 ng,respectively. RSD calculated from peak area of precision,repeatability and stability in 48 h were all less than 3.0%. The average recoveries of timosaponin N,timosaponin L,timosaponin BⅡ,25R-timosaponinBⅡ,and 25S-officinalis-nin-Ⅰwere 98.17%,101.37%,98.53%,97.63%,and 98.17%,respectively. Conclusion The developed method is accurate,reli-able,which could be applied to the quality control of multiple components in A. asphodeloides Bge.
ABSTRACT
Objective: To establish an accelerated solvent extraction (ASE)-charged aerosol detector (CAD) method for simultaneous detection of jujuboside A, jujuboside B, spinosin, and betulinic acid in Zizyphi Spinosae Semen. Methods: The orthogonal design was applied to optimize the extraction parameters of the ASE system. The target compounds were detected by HPLC-CAD with the parameters as follow: Thermo Syncronis C18 (100 mm × 3 mm, 3 μm) column, a gradient elution program with acetonitrile-water as mobile phase at a flow rate of 0.5 mL/min, the column temperature was kept at 40℃. Detector was Corona Ultra CAD with 35℃ of nebulization temperature. Results: Optimization of the ASE parameters with orthogonal design greatly improved the extraction efficiency; All the target compounds could be simultaneously determined in a single run. Good linear relationships (0.998 3-0.999 6) and high relative recoveries were 98.46%-102.02%. Conclusion: The method is rapid, simple, accurate, and thus could be used for the quality control of Zizyphi Spinosae Semen.
ABSTRACT
This paper first briefly introduces the basic information of aminoglycosides for pharmaceutical use such as origin, classification, chemical structures, diversity of composition and the research originators, etc. Then it reviews the development process of the technologies for the analysis of components of aminoglycosides, discusses the advantages and disadvantages of current methodologies and explains the advantage of liquid chromatography coupled with pulsed amperometric detection method for analysis of the components of aminoglycosides. At last, it introduces some new analysis technologies and ideas and forecasts the direction of future development.
ABSTRACT
A high performance liquid chromatography-electrospray ionization mass spectrometry- charged aerosol detection ( HPLC-MS-CAD) method was established for the simultaneous quantitative analysis of four Lignans in Magnoliae Flos extract. The components were separated on a YMC-Pack ODS-A column (250 mm× 4. 6 mm, 5 μm) by gradient elution with methanol and water as the mobile phase at aflow rate of 1. 0 mL/min. Then the elution solution was routed into MS equipment at a flow rate of 0. 3 mL/min and CAD detector at a flow rate of 0. 7 mL/min by a split ratio of 3:7 for the further detection. The column temperature was 25 ℃ and the detection wavelength was 278 nm. A method was developed for the quantitative analysis of muti-components by single maker ( QAMS) to determine pinoresinol dimethylether, magnoli, 1irioresinol B dimethylethe and epi-magnoli A . Magnoli was selected as internal standard and the relative correction factors ( RCF) of the four Lignans were calculated. The contents of the four Lignans in Magnoliae Flos extract were determined by both external standard method and QAMS. The QAMS method was evaluated by comparison of its assay result and that of external standard method. Under the selected chromatographic condition, the limits of detection of pinoresinol dimethylether, magnoli, lirioresinol B dimethylethe and epi-magnoli A were 0. 34, 0. 55, 0. 50 and 0. 58 mg/L, respectively, while the linear range were within 6. 8-270 mg/L, 11-546 mg/L, 2. 0-101 mg/L and 2. 3-116 mg/L. The recoveries ( n=9 ) were 98. 2%-99. 5%, and the correlation coefficient were 0 . 9995-0 . 9998 . No significant differences were found between the quantitative results of external standard method and QAMS method. The developed method is accurate, feasible, and can be used for quality evaluation of Magnoliae Flos .
ABSTRACT
A novel HPLC-CAD method coupled with on-line solid phase extraction ( SPE ) for the determination of erythrocin which was widely used in livestock farming was developed. After mixed with diatomite, 5. 0 g manure sample was put into the cell and extracted with hot water at 70℃ and 10. 3 MPa. An on-line SPE methodology was applied to pre-treat the sample, and the sample was seperated on an Acclaim 120 C18 column and analyzed by corona CAD detector using acetonitrile and 0. 1% formic acid as mobile phase. Good linearity for erythrocin was obtained in the range of 21-2000 μg/kg. The detection limit was 6. 3 μg/kg. The average recoveries were 79. 2%-87. 5%.