Loading...

List of Issues

    Chinese Journal of Chromatography
    2005, Vol. 23, No. 2
    Online: 30 March 2005

    For Selected: Toggle Thumbnails
    研究报告
    Relativity Study on Topological Index of Methylalkane Structures and Chromatographic Retention Index
    XIANG Zheng, LIANG Yizeng, HU Qiannan
    2005, 23 (2):  117-122. 
    Abstract ( 1951 )   [Full Text(HTML)] () PDF (297KB) ( 606 )  
    Quantitative structure-property relationships (QSPR) have been demonstrated to be a powerful tool in chromatography. QSPR have been used to obtain simple models to explain and predict the chromatographic behavior of various classes of compounds. The study of quantitative structure and retention index relationship (QSRR) is an important subject in chromatographic field. One hundred twenty-seven topological descriptors of 207 methylalkane structures are calculated. GAPLS method, which is a variable selection method combining with genetic algorithms (GA), back stepwise and partial least squares (PLS), is introduced in the variable selection of quantitative structure gas chromatographic (GC) retention index relationship. Seven topological descriptors are selected from 127 topological descriptors by GAPLS method to build QSRR model with high regression quality: squared correlation coefficient (R2) of 0.99998, standard deviation (S) of 2.88. The error of the model is similar to the experimental error. The validation of the model is checked by leave-one-out cross-validation technique. The result of leave-one-out cross-validation indicates that the built model is reliable and stable with high prediction quality, such as squared correlation coefficient of leave-one-out (R2cv) of 0.99997 and standard deviation of leave-one-out predictions (Scv) of 2.95. A successful interpretation of the complex relationship between GC retention indexes of methylalkanes and the chemical structure is achieved using QSPR method. The seven variables in the model are also rationally interpreted, which indicates methylalkane retention index are precisely represented by topological descriptors.
    Preparation and Evaluation of 3,5-Dinitrobenzoyl-Bonded Silica Gel Stationary Phase for High Performance Liquid Chromatography
    LI Laisheng, LIU Xu, HUANG Zhibing, GE Xiaohui, LI Yanping
    2005, 23 (2):  123-128. 
    Abstract ( 2428 )   [Full Text(HTML)] () PDF (306KB) ( 678 )  
    A new preparation method of 3,5-dinitrobenzoyl-bonded silica gel stationary phase (DNB) for high performance liquid chromatography has been developed by using N-(β-aminoethyl)-γ-aminopropyl-methyldimethoxy silane as coupling reagent. Its structure was characterized by elemental analysis, diffuse reflectance Fourier transform infrared spectroscopy and thermal analysis. The surface concentration of 3,5-dinitrobenzoyl ligand was 2.08 μmol/m2 according to the carbon content from elemental analysis. The chromatographic performance of the new packing was evaluated by using different solute probes, such as polycyclic aromatic hydrocarbons (PAHs), phenols, naphthalene derivatives, nitrophenol positional isomers and sulfonamides. The results show that comparing with ODS, DNB has weaker hydrophobicity and more versatile chromatographic properties. The charge-transfer between the dinitrobenzoyl ligand and the analytes plays a significant role in the separation of phenols and naphthalene derivatives. In addition, static electric, hydrogen-bonding and dipole-dipole interactions are responsible for the above separations and improve the selectivity of DNB for solutes. An advantage of DNB is that it is suitable for the separation of the basic compounds containing nitrogen atoms without capped process because the spacer containing nitrogen atoms can shield the residual silanols on DNB.
    Studies on Formation of Aggregates from Denatured Lysozymes upon Renaturing with Size Exclusion Chromatography
    BIAN Liujiao, YANG Xiaoyan, LIU Li
    2005, 23 (2):  129-133. 
    Abstract ( 2252 )   [Full Text(HTML)] () PDF (218KB) ( 599 )  
    In order to study the renaturation mechanism of denatured protein in denaturant solution, the renaturation and separation process for three kinds of lysozyme molecules, which were separately denatured by urea and guanidine hydrochloride in the presence of reducing agents, was studied by size exclusion chromatography. When initial lysozyme concentration in denaturant solution was more than 10 g/L, the denatured lysozyme molecules were renatured and isolated in a size exclusion chromatographic column. A refolded lysozyme intermediate, a bi-molecular aggregate, was found. This result was confirmed by non-reducing sodium dodecyl sulfate-polyacrylamide gel electrohoresis (SDS-PAGE) analysis of renatured lysozyme molecules with the dilution method. Compared with the dilution method, the amount of the bi-molecular aggregate found by size exclusion chromatography was far less than that found in the dilution method. This result shows that the process for the renaturing of denatured lysozyme molecules in solution can be well described with three-state model in the presence of reducing agents.
    Studies on Immunoaffinity Chromatography for Carbofuran
    LIU Shuzhao, WEI Linhong, XU Weina
    2005, 23 (2):  134-137. 
    Abstract ( 2192 )   [Full Text(HTML)] () PDF (186KB) ( 816 )  
    The purified anti-carbofuran antibody was conjugated to carbonyl diimidazole (CDI)-activated Sepharose CL-4B to synthesize the immunosorbent for the immunoaffinity chromatographic (IAC) column specific to carbofuran. The conditions of IAC were optimized as follows: pH 7.2 phosphate buffer (PB) was used as equilibrium and adsorbent medium, and methanol-water (60∶40, v/v) as eluent. The results showed that the dynamic column capacity was up to 1.58 mg/L bed volume. The efficiency of enrichment of IAC was more than 167 times when the initial concentration of carbofuran in a standard sample solution was lower than 2 μg/L. The spiked river water was cleaned up and enriched by IAC, and carbofuran in eluate was determined by enzyme linked immunosorbent assay (ELISA). The average recovery of carbofuran from river water was 89.8% with the relative standard deviation of 4.8% at the spiked level of 0.1 mg/L. Meanwhile the eluate was determined by high performance liquid chromatography (HPLC), the results from HPLC correlated well with those from ELISA. The IAC method of carbofuran was successfully established.
    Study on the Simultaneous Determination of 7-Methylguanosine and Mitomycin C by Capillary Electrophoresis with Amperometric Detection
    ZHANG Lan, HE Yu, CHEN Yiting, TONG Ping, CHEN Guonan
    2005, 23 (2):  138-141. 
    Abstract ( 2238 )   [Full Text(HTML)] () PDF (188KB) ( 629 )  
    A method based on capillary electrophoresis with amperometric detection (CE-AD) has been developed for the simultaneous determination of 7-methylguanosine and mitomycin C. The detection electrode was a 0.3 mm carbon disc electrode at a working potential of 950 mV (versus Ag/AgCl electrode). A suitable electrolyte consists of 20 mmol/L phosphate buffer (pH 9.4), with the separation voltage of 18 kV, the injection time of 10 s, and the injection voltage of 18 kV. Under optimum conditions, the two analytes could be well separated within 10 min in a 60 cm length capillary. The current responses were linear over about two orders of magnitude (0.50-50 mg/L) with detection limits (S/N=3) of 0.050 and 0.025 mg/L for 7-methylguanosine and mitomycin C, respectively. The proposed method was successfully applied to determine the synthetic urine and serum samples. The recoveries were found in the range of 93.0%-97.2%.
    Communications
    Analysis of Positional Distribution of Fatty Acids in Triacylgly-cerols from Lard by High Performance Liquid Chromatography
    ZHAO Haizhen, LU Zhaoxin, BIE Xiaomei, L Fengxia
    2005, 23 (2):  142-145. 
    Abstract ( 2600 )   [Full Text(HTML)] () PDF (170KB) ( 1342 )  
    A high performance liquid chromatographic (HPLC) method for the determination of fatty acid positional distribution on triacylglycerols from lard has been established. The analysis was carried out with an sn-1, 3 specific lipase to deacylate the fatty acid residues esterified at sn-1 and sn-3 positions of triacylglycerols, forming sn-2 monoglycerides and free fatty acids. After lipase action, it was possible to determine the fatty acid esterified at the sn-2 position by the substraction of the results of the sn-1,3 analysis from an overall composition analysis based on complete saponification of the original sample. The free fatty acid mixtures were converted to phenacyl esters via 2-bromoacetophenone and analyzed on an Agilent 1100 series high performance liquid chromatograph, equipped with a ZORBAX SB C18 column (4.6 mm i.d.×250 mm, 5 μm) and a UV detector. Elution was performed at a flow rate of 1 mL/min, with a gradient of methanol-acetonitrile-water starting at 80∶10∶10 (v/v), increasing linearly to 86∶10∶4 (v/v) in 35 min, then returning to the initial conditions in 5 min. Elution of phenacyl esters was monitored by absorbance at 254 nm. Pentadecanoic acid was used to be an internal standard. The results showed that palmitic and oleic acids were the major components in lard, accounting for 26.61% and 43.18% respectively. Among these, palmitic acid mainly locates at sn-2 position, while oleic acid at sn-1,3 positions. These results were consistent with those obtained via gas chromatographic method. The new method is simpler and easier to use as it eliminates time-consuming thinner-layer chromatography used in standard regioselective analysis. It is possible to be an effective laboratory analytical method.
    Reviews
    Application of Binaphthyl Derivatives as Chiral Stationary Phases in High Performance Liquid Chromatography
    LIU Xudong, DING Jinying, GAO Lianxun
    2005, 23 (2):  146-151. 
    Abstract ( 2135 )   [Full Text(HTML)] () PDF (270KB) ( 1205 )  
    Optically active axially dissymmetric binaphthyl derivatives have been extensively used as excellent chiral ligands in asymmetric catalysis and chiral recognition. The review describes the applications of binaphthyl derivatives as chiral stationary phases in high performance liquid chromatography. Fifty four references are cited.
    Capacitively Coupled Contactless Conductivity Detection in Capillary Electrophoresis
    TAN Feng, GUAN Yafeng
    2005, 23 (2):  152-157. 
    Abstract ( 3150 )   [Full Text(HTML)] () PDF (254KB) ( 963 )  
    Capacitively coupled contactless conductivity detection (C4D) is a new detection technique has been developed in recent years and used mainly in capillary electrophoresis and microchip electrophoresis. The characteristics of C4D detector are simple in structure, easy in miniaturization and integration, and free of electrodes contamination, which are common problems in an electrochemical detection. The principles and progresses of C4D in capillary electrophoresis are reviewed.
    研究简报
    Similarity System Theory to Evaluate Similarity of Chromatographic Fingerprints of Traditional Chinese Medicine
    LIU Yongsuo, MENG Qinghua, JIANG Shumin, HU Yuzhu
    2005, 23 (2):  158-163. 
    Abstract ( 2441 )   [Full Text(HTML)] () PDF (224KB) ( 1127 )  
    The similarity evaluation of the fingerprints is one of the most important problems in the quality control of the traditional Chinese medicine (TCM). Similarity measures used to evaluate the similarity of the common peaks in the chromatogram of TCM have been discussed. Comparative studies were carried out among correlation coefficient, cosine of the angle and an improved extent similarity method using simulated data and experimental data. Correlation coefficient and cosine of the angle are not sensitive to the differences of the data set. They are still not sensitive to the differences of the data even after normalization. According to the similarity system theory, an improved extent similarity method was proposed. The improved extent similarity is more sensitive to the differences of the data sets than correlation coefficient and cosine of the angle. And the character of the data sets needs not to be changed compared with log-transformation. The improved extent similarity can be used to evaluate the similarity of the chromatographic fingerprints of TCM.
    Separation and Identification of Metallothionein Isoforms and Sub-isoforms by Liquid Chromatography
    LU Suge,SHEN Jincan,ZHUANG Zhixia,WANG Xiaoru,
    2005, 23 (2):  164-167. 
    Abstract ( 1888 )   [Full Text(HTML)] () PDF (197KB) ( 846 )  
    A method has been established for the separation and identification of metallothionein (MT) isoforms and sub-isoforms by liquid chromatography. A mixture of rabbit liver MT was separated on a DEAE A-25 weak anion-exchange chromatographic (AEC) column. Inductively coupled plasma-mass spectrometer (ICP-MS) was used for off-line detection of Zn in each fraction. The two main MT isoforms, MT-1 and MT-2, were isolated. The collected MT isoform fractions were then desalted by a homemade Sephadex G-25 size exclusion chromatographic (SEC) column. Afterwards, the sample was separated on a C18 reversed-phase column with UV detection at 210 nm. Different separation conditions were discussed and several sub-isoforms of MT were well separated at pH 2.0. The sub-isoforms were finally characterized by on-line HPLC-ESI-MS. The isoforms and sub-isoforms were well separated on a reversed-phase column under optimized chromatographic conditions and the detection results of ESI-MS were in agreement with the data found in literature. The method developed can be well used for the separation of metallothionein isoforms and sub-isoforms.
    Separation of Interleukin-18 on a Weak Anion Exchange Monolithic Column
    ZHAO Jumin, YANG Gengliang, ZHENG Chao, LIU Haiyan, WANG Manman, CHEN Yi
    2005, 23 (2):  168-171. 
    Abstract ( 1914 )   [Full Text(HTML)] () PDF (191KB) ( 697 )  
    A weak anion exchange column was prepared and a separation method of interleukin-18 (IL-18) was developed on the column. The chromatographic column with glycidyl methacrylate as functional monomer and ethylene dimethacrylate as cross-linker was prepared by a free radical polymerization within a 64 mm×4.6 mm i.d. column. The epoxide groups of the column were modified by a reaction with diethylamine that affords ionizable functionalities required for ion exchange chromatography. The influences of the contents of the cross-linker and porogen on column pressure were investigated. The factors influencing the separation, such as stationary phases, buffers, pH values, salts, and contents of organic solvent, were studied. The optimal conditions for separating IL-18 from its related proteins were obtained. The proposed method is simple, sensitive, rapid and reproducible.
    Study of Enantiomeric Separation of DL-Amino Acids on L-Isoleucine-Type Chiral-Ligand-Exchange Stationary Phase
    HUANG Xiaojia, WANG Qiuquan, WANG Junde, HUANG Benli
    2005, 23 (2):  172-175. 
    Abstract ( 2308 )   [Full Text(HTML)] () PDF (193KB) ( 663 )  
    Some underivatized DL-amino acid enantiomers were separated on L-isoleucine-type chiral-ligand-exchange stationary phase (EILE). The effects of contents of copper ion and methanol in mobile phase, temperature of column and flow rate of eluent on the efficiency and resolution of DL-amino acids were investigated in detail. The results showed that Cu(Ⅱ) ion played an important role in the separation. When there was no Cu(Ⅱ) ion in mobile phase, the DL- amino acids could not be enantio-separated, while the content of Cu(Ⅱ) increased from 0.3 mmol/L to 1.2 mmol/L, the efficiency of resolution and retention time decreased. The increases of the content of methanol and column temperature are in favor of the resolution for most of DL-amino acids. The flow rate also affected the resolution results. Good results could be obtained in reducing flow rate but it prolongs the retention time. The mechanisms of different chiral separation results on the new stationary phase under different conditions were also investigated.
    Determination of Estrogen-Like Compounds in Beverages by High Performance Liquid Chromatography
    HAN Hao, SHAO Bing, MA Yalu, WU Guohua, XUE Ying
    2005, 23 (2):  176-179. 
    Abstract ( 2023 )   [Full Text(HTML)] () PDF (213KB) ( 776 )  
    A comprehensive analytical method based on high performance liquid chromatography-ultravioiet-fluorescence detection (HPLC-UV-FL) has been established for the determination of bisphenol A (BPA), nonylphenol (NP) and octylphenol (OP) in beverages with different samples and concentrations. Clean-up of samples was performed on an OASIS HLB solid extraction cartridges (6 mL, 200 mg). The method was successfully applied to the investigation of residual bisphenol A, nonylphenol and octylphenol in the beverages (mineral waters and soft drinks) available in commercial markets in Beijing. Recoveries for bisphenol A, nonylphenol and octylphenol at different spiked levels were ranged from 91.08% to 103.19% with relative standard deviations of 0.5% to 5.49%. The method is simple with good reproducibility and selectivity, and high sensitivity.
    Determination of p-Coumaric Acid in Hedyotis diffusa Willd. from Different Sources by Reversed-Phase High Performance Liquid Chromatography
    ZHANG Caihua, GUO Xingjie, BAO Ludan, QIN Feng, LI Famei
    2005, 23 (2):  180-182. 
    Abstract ( 2105 )   [Full Text(HTML)] () PDF (164KB) ( 712 )  
    A method for the determination of p-coumaric acid in Hedyotis diffusa Willd. from different sources by reversed-phase high performance liquid chromatography (RP-HPLC) has been developed. p-Coumaric acid was successfully separated on a DiamonsilTM ODS column (4.6 mm i.d.×250 mm, 5 μm) at ambient temperature, using a mixture of CH3CN-20 mmol/L NH4Ac (pH 4.0) (15∶85, v/v) as mobile phase and detection at 308 nm. The flow rate was 1.0 mL/min. There was good linear relationship (r=0.9996) between the mass concentration and the peak area of p-coumaric acid in the range of 4.04-202 mg/L. The recoveries were found to be in the range of 97.4%-102.2%. The results of the experiments have demonstrated that the established method is rapid and simple with good accuracy and reproducibility. The method is suitable for use in quality control of Hedyotis diffusa Willd. from different sources.
    Quantitative Analysis of Complicated Casein Hydrolysates by High Performance Size Exclusion Chromatography
    YU Yanjun, QI Wei, HE Zhimin
    2005, 23 (2):  183-185. 
    Abstract ( 2225 )   [Full Text(HTML)] () PDF (142KB) ( 667 )  
    The enzymatic hydrolysates of casein are so complicated that there has no effective method for quantitative analysis. On the basis of membrane separation and high performance size exclusion chromatography (HPSEC), standard peptides with different relative molecular mass ranges were prepared, and the linear relationships between mass concentration of the standard peptides and the corresponding peak areas were established. Consequently, mass concentration of the different hydrolysates at different reaction time can be accurately calculated. The combination of chromatography and membrane separation is of great importance to the quantitative analysis of the complicated hydrolysates, which can be also applied to the other macromolecular systems, such as carbohydrates.
    Study on Drug Displacement Interactions by Capillary Electrophoresis-Frontal Analysis
    ZHOU Dawei, WANG Huaifeng, LI Famei
    2005, 23 (2):  186-188. 
    Abstract ( 2744 )   [Full Text(HTML)] () PDF (150KB) ( 703 )  
    The interaction between 18-methyl norethindrone and ketoprofen including the displacement of ketoprofen from human serum albumin binding sites was investigated by capillary electrophoresis-frontal analysis method (CE-FA) at room temperature. A very large sample plug was introduced hydrostatically into the capillary (65 cm×50 μm i.d., effective length of 35 cm) over 80 s at a height difference of 11 cm. The working conditions for CE-FA separation are as follows: operating voltage, 10 kV; running buffer, 67 mmol/L phosphate, pH 7.4. The unbound ketoprofen concentration was directly measured from the height of the frontal peak. When the concentration of 18-methyl norethindrone was increased from 0 to 200 μmol/L, the unbound ketoprofen concentration was found to increase from 22.4 to 26.4 μmol/L at 100μmol/L total ketoprofen concentration and from 82.1 to 106.2 μmol/L at 200 μmol/L total ketoprofen concentration. From these data, it may be deduced that the administration of high concentration of 18-methyl norethindrone could displace ketoprofen from its secondary binding site.
    Study on Characteristics of Bias Caused by Flow Injection-Capillary Electrophoresis with
    LUO Jinwen, ZHU Hailin, LI Huilin
    2005, 23 (2):  189-192. 
    Abstract ( 2106 )   [Full Text(HTML)] () PDF (176KB) ( 736 )  
    The characteristics of bias caused by split-flow electrokinetic injection (SEKI), a new sample injection method applied in coupled flow injection-capillary electrophoretic system(FI-CE), was investigated using pseudoephedrine hydrochloride, a basic drug and ibuprofen, an acidic drug, as model analytes. It was found that bias imposed by SEKI under the conditions of continuous sample matrix/running buffer was similar to that did by electrokinetic injection (EKI). The linearity of calibration curve provided by SEKI was similar to that offered by non-bias hydrodynamic injection (HDI) but significantly better than that obtained by EKI. These features were exploited to improve analytical performances in simultaneous determination of the minor ingredient of pseudoephedrine hydrochloride and the major ingredient of ibuprofen in pharmaceutical preparation. Detectability of 0.7 mg/L for pseudoephedrine hydrochloride, was achieved at a sample throughput rate of 24 times per hour which is 30% lower than that obtained by HDI-based conventional CE. Eleven runs of a test solution containing 13.1 mg/L pseudoephedrine hydrochloride and 81.4 mg/L ibuprofen produced relative standard deviations (RSDs) of 2.8% for the minor ingredient and 1.2% for the major ingredient, which were improved in comparision to that obtained by HDI-based conventional CE. Analytical results for two batches of compound ibuprofen tablets by the SEKI-based FI-CE approach were in good agreement with that obtained by a conventional high performance liquid chromatographic method.
    Analysis of Fatty Acids in Tissues of Penaeus vannamei Cultured in Sea- and Fresh-Waters by Ultrasonic Extraction-Capillary Gas Chromatography
    LU Jie, HUANG Kai, ZANG Ning, LI Junfang, ZHANG Min, WANG Yong
    2005, 23 (2):  193-195. 
    Abstract ( 2244 )   [Full Text(HTML)] () PDF (154KB) ( 745 )  
    The components and contents of fatty acids in the muscle and the hepatopancreas of Penaeus vannamei cultured in the ponds of sea- and fresh-waters were determined. Lipid was extracted from tissues with “Folch” solvent under ultrasonication, and esterified with KOH-BF3 method followed by capillary gas chromatography. A fused-silica BPX70 capillary column (60 m×0.25 mm i.d.) and flame ionization detector (FID) were employed. Fatty acids, more importantly, the positional isomers, were identified by applying equivalent chain length (ECLT) values based on even-chain saturated fatty acid methyl ester standards. Area normalization method can be used to quantify the contents of the fatty acids. The results indicated that between the two kinds of shrimps the nature of major fatty acids were the same, but there were more differences in the contents of major fatty acids. In all the tested fatty acids, the unsaturated fatty acids (UFA) were majority and the contents of polyunsaturated fatty acids were obviously higher than monounsaturated fatty acids. In the muscle lipid of the two kinds of shrimps, the total contents of eicosapentaenoic acid (EPA) and docosahexenoic acid (DHA) (highly unsaturated fatty acids) were very high, which reached to over 20%. In the hepatopancreas, the total contents of EPA and DHA were lower (ranged from 11% to 17%). Contents of n-6 cluster UFA in fresh-water shrimps were higher than that in sea-water shrimps. The value of (n-3)/(n-6) of sea-water shrimps was higher than that of fresh-water shrimps.
    Analysis of the Volatile Oil from the Stem of Acanthopanax senticosus (Rupr. et Maxim.) Harms with Several Hyphenated Methods of Gas Chromatography
    YU Wanying, ZHANG Hua, HUANG Weidong, CHEN Jiping, LIANG Xinmiao
    2005, 23 (2):  196-201. 
    Abstract ( 2085 )   [Full Text(HTML)] () PDF (333KB) ( 551 )  
    Gas chromatography/quadrupole mass spectrometry(GC/qMS), gas chromatography/Fourier transform infrared spectrometry (GC/FTIR) and gas chromatography/orthogonal acceleration time-of-flight mass spectrometry (GC/oaTOFMS) were applied to analyze the volatile oil from the stem of Acanthopanax senticosus ( Rupr. et Maxim.) Harms. Based on the spectra search function of GC/qMS with the aid of the discriminability of the geometrical isomer by GC/FTIR and the ability to determine the accurate mass charge ratio (m/z) by GC/oaTOFMS, 68 GC eluants were identified successfully. Compared with the results obtained by GC/qMS only, the analytical results obtained by these hyphenated methods of gas chromatography are more reliable.
    Determination of the Writing Age of Blue Ballpoint Ink by Gas Chromatography
    WANG Yan, YAO Lijuan, ZHAO Pengcheng, WANG Jinghan, WANG Yanji
    2005, 23 (2):  202-204. 
    Abstract ( 2087 )   [Full Text(HTML)] () PDF (140KB) ( 926 )  
    A method of identifying the writing age of blue ballpoint ink has been established for imperative demand of forensic laboratory. The content of the volatile component in blue ballpoint ink was determined by gas chromatography (GC). The absorbance of the dye in the blue ballpoint ink was measured by ultraviolet-visible spectrometry (UV-Vis). A writing age curve of the blue ballpoint ink has been established by the ratio of the content of the volatile components and the dye, based on the identification of 74 kinds of blue ballpoint inks, from both domestic and international origins. The change of benzyl alcohol or phenoxyethyl alcohol was tested with the writing age. Blue ballpoint inks of different kinds were detected and the repeatability of the experiment was investigated. The results indicated that the method is reliable and systematic, and especially suitable for practical cases.
    Simultaneous Determination of Cl- and SO2-4 in 30% Sodium Bisulfite Solution Samples by Ion Chromatography
    LU Keping
    2005, 23 (2):  205-207. 
    Abstract ( 2374 )   [Full Text(HTML)] () PDF (151KB) ( 968 )  
    A novel method for simultaneous determination of Cl- and SO2-4 in 30% sodium bisulfite solution samples by ion chromatography was established. A sample was pretreated with triethanolamine (TEA) to prevent sulfite from becoming sulfate. The mixture solution of 1.5 mol/L Na2CO3-3.5 mol/L NaHCO3-10% (v/v) (CH3)2CO was used as eluent with a flow rate of 1.0 mL/min. The injection volume was 25 μL. The separation was performed on an IonPac AS14 column and detected by suppressed conductivity with external acid mode. Both Cl- and SO2-4 have good linearity in the ranges of 0.05-1.5 mg/L and 0.20-15 mg/L with correlation coefficients above 0.999 and the detection limits of Cl- and SO2-4 were 0.01 and 0.03 mg/L, respectively. The proposed method is simple and rapid and has been successfully applied to the analysis of 30% sodium bisulfite samples. The entire process of analysis is completed within 12 min.