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作 者:杨辉 潘建斌[2] 谢咏诗[2] 李新春[3] 陈缵光[2]
机构地区:[1]广西分析测试研究中心,广西南宁530022 [2]中山大学药学院医药仪器与应用研究所,广东广州510006 [3]广西医科大学药学院药物分析教研室,广西南宁530021
出 处:《分析测试学报》2013年第4期473-477,共5页Journal of Instrumental Analysis
基 金:国家自然科学基金资助项目(21075139);广西医科大学青年科学基金资助项目(GXMU YSF201204)
摘 要:报道了一种芯片毛细管电泳-非接触电导法,用于快速测定葡萄糖氯化钠注射液中两种药物的含量。实验考察了运行缓冲液pH值和分离电压对组分分离的影响,以及检测器激励频率对组分信号响应和灵敏度的影响。确定以20 mmol/L硼酸缓冲液(pH 9.6)为分离介质,分离电压为1 200 V;最佳激励频率为70kHz。在上述条件下,两种成分(葡萄糖和Na+)可在60 s内实现有效分离。Na+和葡萄糖的线性响应范围分别为20~1 000μmol/L和50~5 000μmol/L(r≥0.992);按信噪比(S/N)为3∶1计算检出限分别为8.2μmol/L和26.7μmol/L。两个组分的回收率分别为95%~99%和97%~104%,相对标准偏差(RSDs)均小于4.0%。该文首次报道了葡萄糖和氯化钠两种常见药物成分的同时测定。方法简便、快速、准确度高、稳定性好,用于注射剂含量的测定,结果满意。A microchip capillary electrophoresis with contactless conductivity detection method was developed for the rapid determination of glucose and sodium chloride in the injection preparation. The pH value and constituent of running buffer were investigated to gain the effective resolution of the two ingredients. The excitation frequency of the detector was also surveyed in view of the signal response and detection sensitivity. The optimal conditions were as follows: separation media: 20 mmmol/L borate(pH 9.6), separation voltage : 1 200 V, excitation frequency : 70 kHz. Under the optimal conditions, the two analytes could be successfully separated within 60 s. Good linearities (r ≥0. 992) for NaCl and glucose were obtained in the ranges of 20 - 1 000 txmol/L and 50 - 5 000μmol/L, respectively. The limits of detection ( S/N = 3 : 1 ) were 8.2 μmol/L and 26. 7 μmol/L, respectively. The spiked recoveries for Na+ and glucose were 95% - 99% and 97% - 104% , re- spectively, with relative standard deviations ( RSDs, n = 3 ) less than 4. 0% . The present work pro- vided an approach of choice to the simultaneous quantitative analysis of glucose and NaC1 in the com- pound preparation widely used in clinical therapeutics. With the advantages of convenience, rapidi- ty, considerable accuracy and stability, this method was applied in the determination of Na+ and glucose in real sample with satisfactory result.
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