| Ion chromatography is a well-established analytical method for detecting anions and cations in food,environmental,clinical,pharmaceutical and many other samples.In this work,analytical methods for the determination of organic and inorganic anions in pharmaceuticals and cultured cell samples by ion chromatography were developed.The main contents and results are the following:(1)New method for the detection of cyanide in drugs with complex matrix by ion chromatography with amperometric detector was established.For sample preparation procedure,drug samples were heated and distilled in a phosphoric acid solution,and the hydrogen cyanide was evaporated and absorbed by the sodium hydroxide solution.The method has the advantage of avoiding the interference of matrix in samples and was successfully applied for the detection of cyanide in pharmaceutical formulation samples.The analytical column IonPac AS11-HC protected with IonPac AG11-HCwas used for separations and NaOH 4mmol/L was used as the mobile phase.The linear relationship of CN-was excellent in the range from 0.02 to 1.0 mg/L with correlation coefficient of 0.9993.LOD for CN-was 0.10μg/gand the recovery results ranged from 96.0%to 101.1%.The method revealed high sensitivity,high precision and good repeatability.(2)The new analytical method for determination of EDTA in pharmaceutical formulations by ion chromatographic with conductivity detector was developed.The method was validated in terms of accuracy,precision,and sensitivity.Dissolution was the only sample preparation method used during this study.The detection of this chelating agent(EDTA)in pharmaceutical samples by ion chromatography method is sensitive(LOD was 0.02mg/L),fast and accurate.The results also showed excellent recoveries(87.8-99.8%),high precision(RSD<0.31%),and excellent linearity(R=0.99998).Therefore,the developed method is suitable for determination of EDTA in complex biological samples.(3)A novel detection method based on ion chromatography with conductivity detector was developed for a simultaneous quantification of low molecular weight organic acids such as α-ketoglutarate,oxalate,fumarate and citrate in Botrytis cinerea.The samples were diluted 10-fold with ultrapure water and filtered through 0.22 μm PTFE membrane for further IC analysis.By using a gradient solution of KOH as the mobile phase and IonPacAS18 as analytical column,the efficient resolution was obtained from possible coexisting anions such as acetate,carbonate ion,tartrate and isocitrate.The developed method was applied for organic acids detection with simple sample preparation,an excellent linearity(r2>0.999),good recoveries(74.7-97.8%),excellent repeatability(RSD<4%)and low limit of detections(LOD)ranging from 0.0015 to 0.003mg/L.(4)An efficient new detection method based on ion chromatography with conductivity detection was developed for a simultaneous determination of oxalate,α-ketoglutarate,fumarate and citrate in hemocytes of Mythimna separata larvae.Before being injected into ion chromatography system,the samples were diluted 10-fold with ultrapure water and filtered through 0.22 μm PTFE membrane.The method was applied by using thelonPac AS 18 column with a mobile phase containing a gradient solution of KOH.Recovery study was performed and satisfactory recoveries between 85.03%and 107.6%for all studied organic acids were obtained.The four organic acids were quantitatively determined simultaneously in the immuno-hemocytes.The developed method has high accuracy,excellent repeatability and selectivity,which is suitable for the separation and determination of organic acids in hemocytes so as to monitor cellular immunity.The different action characteristics of an anticancer quinazoline drug and an insecticide emamectin benzoate on the hemocytes from Mythimna separta larvae were well revealed. |
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