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目的:建立高效毛细管电泳测定匹伐他汀钙中(-)-(3S,5R)-对映体含量的方法。方法:研究影响对映体拆分的手性选择剂的种类及浓度、缓冲液的浓度和pH、电泳工作电压、温度,选出手性拆分的最佳条件,采用未涂层毛细管柱(57 cm×75μm,有效长度为50 cm),用50 mmol·L-1磷酸二氢钠溶液(用磷酸调节pH至3.0,含有50 mmol·L-1γ-环糊精)作为填充缓冲液;50 mmol·L-1的磷酸二氢钠溶液(用磷酸调节pH至3.0)作为运行缓冲液;工作电压为20 kV,分离温度为20℃;压力进样方式,进样压力为3.4 kPa,时间为5 s;检测波长为245 nm。结果:匹伐他汀钙2个对映异构体达到基线分离,迁移时间和峰面积的RSD小于2%,最低检测限为0.1μg·mL-1。结论:采用本方法可简便、准确地测定匹伐他汀钙中(-)-(3S,5R)-对映体的含量。
Objective: To establish a method for determination of (-) - (3S, 5R) - enantiomer in pitavastatin calcium by high performance capillary electrophoresis. Methods: The types and concentrations of chiral selectors influencing the resolution of enantiomers, the concentration and pH of the buffer, the operating voltage and the temperature of the electrophoresis were investigated. The optimal conditions for the chiral resolution were selected. The uncoated capillary column cm × 75μm, the effective length of 50 cm), with 50 mmol·L-1 sodium dihydrogen phosphate solution (pH adjusted to 3.0 with phosphoric acid, containing 50 mmol·L -1 γ-cyclodextrin) as a filling buffer; 50 mmol · L-1 sodium dihydrogen phosphate solution (adjusted to pH 3.0 with phosphoric acid) as running buffer; working voltage is 20 kV, separation temperature is 20 ℃; pressure injection mode, injection pressure is 3.4 kPa, time is 5 s; detection wavelength is 245 nm. Results: The two enantiomers of pitavastatin reached baseline separation, the RSD of migration time and peak area was less than 2%, and the lowest detection limit was 0.1 μg · mL-1. Conclusion: This method can be used to determine the content of (-) - (3S, 5R) - enantiomer in pitavastatin calcium easily and accurately.