流动注射-毛细管电泳分流式电动进样歧视效应特征的研究

以碱性药物盐酸伪麻黄碱和酸性药物布洛芬为对象研究了分流式电动进样(一种用于流动注射-毛细管电泳(FI-CE)联用系统的新进样方法)歧视效应的特性。结果发现:在样品介质与运行缓冲液一致的条件下,FI-CE分流式电动进样产生的歧视效应与电动进样相似,但获得的校正曲线的线性明显优于电动进样,而与没有歧视效应的压力进样所获得的线性相似。利用这些特征提高了同时测定复方布洛芬片中少量组分盐酸伪麻黄碱和主要组分布洛芬的分析性能。在24次/h的采样频率下,盐酸伪麻黄碱的检测限为0.7 mg/L,比采用压力进样的毛细管电泳法所得的检测限低30%。连续进样11次分析含有13.1 mg/L盐酸伪麻黄碱和81.4 mg/L布洛芬的试样溶液,峰面积的相对标准偏差分别为2.8%(盐酸伪麻黄碱)和1.2%(布洛芬),明显优于采用压力进样的毛细管电泳法。用该法测定了两批复方布洛芬片中两种组分的含量,所得结果与高效液相色谱法的测定结果一致。

Study on Characteristics of Bias Caused by Flow Injection-Capillary Electrophoresis with

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. )