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    高精度胶束毛细管电动色谱法测定牛磺酸滴眼液中牛磺酸和羟苯乙酯的含量

    Determination of Taurine and Ethylparaben in Taurine Eye Drops by High-Precision Micellar Capillary Electrokinetic Chromatography

    • 摘要: 建立了高精度胶束毛细管电动色谱法同时测定牛磺酸滴眼液中牛磺酸和羟苯乙酯含量的方法。移取牛磺酸滴眼液样品5.0 mL,用水定容至10 mL,超声混匀,经0.22 μm微孔滤膜过滤,取续滤液,得到待测样品溶液。选择带隔离槽的石英毛细管柱(内径75 μm,总长度65 cm,有效长度45 cm),以含20 mmol·L-1十二烷基硫酸钠的硼砂-硼酸缓冲液(pH 9.0,15 mmol·L-1)的混合液为分离缓冲液,在分离电压为-15 kV,检测波长为210 nm的条件下进行电泳分离。结果显示:牛磺酸的质量浓度在5.02~40.80 g·L-1内,羟苯乙酯质量浓度在0.050~0.333 g·L-1内与其各自对应的峰面积呈线性关系,检出限分别为1.2,0.005 g·L-1;牛磺酸和羟苯乙酯混合标准溶液的日内精密度(n=6)均小于2.0%,日间精密度(n=6)均小于4.0%;对实际样品进行加标回收试验,牛磺酸的回收率为93.9%~111%,羟苯乙酯的回收率为85.3%~107%。方法用于3批牛磺酸滴眼液的分析,牛磺酸和羟苯乙酯的测定值与其标示量基本一致。

       

      Abstract: A method for simultaneous determination of taurine and ethylparaben in taurine eye drops by high-precision micellar capillary electrokinetic chromatography was established. 5.0 mL of taurine eye drops sample was made its volume up to 10 mL with water. The subsequent filtrate was obtained as sample solution for test affer mixing ultrasonically and filtrating through 0.22 μm microporous membrance. A quartz capillary column with isolation tank (75 μm of inner diameter, 65 cm of total length and 45 cm of effective length) was selected, and a mixture of borax and boric acid buffer (pH 9.0, 15 mmol·L-1) containing 20 mmol·L-1 sodium dodecylsulfate was used as separation buffer reagent. Electrophoretic separation was carried out at -15 kV of separation voltage and 210 nm of detection wavelength. As shown by the results, linear relationships between mass concentrations of taurine and ethylparaben and their peak areas were kept in the ranges of 5.02-40.80 g·L-1 and 0.050-0.333 g·L-1, with detection limits of 1.2 g·L-1 and 0.005 g·L-1, respectively. Intra-day precision (n=6) of mixed standard solution of taurine and ethylparaben were less than 2.0%, and inter-day precision (n=6) were less than 4.0%. Recovery test was made on substantial sample by standard addition method, and values of recovery were in the ranges of 93.9%-111% for taurine and 85.3%-107% for ethylparaben. This method has been applied for analysis of 3 batches of the taurine eye drops, and the determined values of taurine and ethylparaben were basically consistent with their labeled amounts.

       

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