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作 者:方晓明[1] 谢征宇[1] 叶建农[1] 方禹之[1]
机构地区:[1]华东师范大学化学系
出 处:《色谱》1996年第6期467-469,共3页Chinese Journal of Chromatography
基 金:中科院长春应用化学研究所电分析化学开放实验室资助
摘 要:用高效毛细管电泳-安培检测装置,以200μm铜圆盘电极为工作电极,在碱性介质中,建立了分离测定丙三醇和山梨醇的最佳实验条件。结果表明:平均理论塔板数为2.4×105/m,丙三醇和山梨醇的浓度检测限分别为300μg/L和200μg/L,线性范围接近3个数量级。在5.00~50.0mg/L内,丙三醇和山梨醇的相关系数分别为0.9997和0.9995。样品测定结果与用高效液相色谱法测定的结果基本一致。Capillary zone electrophoresis coupled with amperometric detection by using a copper electrode, was employed for the determination of glycerol and sorbitol in tooth paste samples. The electrode used was a 200μm diameter Cu disk electrode operated in a wall jet configuration with an applied potential of +0.65V (vs. Ag/AgCl) and 80cm capillary (o.d. 360μm, i.d. 25μm) at 30kV in the electrophoretic medium of 0 10mol/L NaOH. Glycerol and sorbitol could be completely separated within 10 min. The detection limits, based on a signal to noise ratio of 3, were about 300μg/L for glycerol and 200μg/L for sorbitol, or corresponding to 1.4pg and 0.96pg respectively calculated from the migration time of glycerol with an injection volumn of 4.8nL. The linear dynamic ranges were from the detection limits up to 100mg/L, and within the range of the linearity, calibrations were performed by injection of a set of standards of the mixed solutions varying from 5.00mg/L to 50.0mg/L,giving the following equations of regression lines as well as regression coefficients for glycerol and sorbitol, respectively: H(cm)=0.56 + 0.31C(mg/L) (r=0.9997) and H(cm)=1.33 +0.77C(mg/L) (r=0.9995). The reproducibility of response was tested by 11 repetitive injections of 10.0mg/L of a mixed solution, and the RSD of the peak current was about 2.2% for glycerol and 2.5% for sorbitol. The analytical results of the tooth paste samples were very close to the contents gained by the HPLC method, and the recovery were in the range of 92% 104%. The method is simple, rapid and highly reliable for routine analysis of underivatized polyols in tooth paste.
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