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采用胶束扫集毛细管电动色谱技术,建立了测定药物中邻苯二甲酸二甲酯(DMP)、邻苯二甲酸二乙酯(DZP)和邻苯二甲酸二丁酯(DBP)的方法。电泳缓冲体系含80 mmol/L SDS,20 mmol/L NaH2PO4(pH 2.20),5%甲醇(V/V),分离电压-18 kV,重力进样80s×15.0cm,检测波长225 nm,使用Φ50μm×62.0 cm石英毛细管,有效长度50.0 cm。讨论了磷酸盐浓度、有机改善剂、SDS浓度、分离电压、进样时间等因素的影响,并考察了胶束扫集法对DMP、DEP和DBP的富集能力。在优化条件下,线性关系良好,相关系数大于0.9986,DMP、DEP和DBP的线性范围分别为1.25～240,1.04～200和1.56～200 mg/L,检出限分别为0.26,0.26和0.39 mg/L。方法应用于肠溶片中DMP、DEP和DBP的测定,回收率在93.3%～108%之间,RSD≤5.2%。每次样品测定可在10 min内完成。
A method for the determination of dimethyl phthalate (DMP), diethyl phthalate (DZP) and dibutyl phthalate (DBP) in pharmaceuticals was established using micellar scanning capillary electrokinetic chromatography. The electrophoresis buffer system consisted of 80 mmol / L SDS, 20 mmol / L NaH2PO4 (pH 2.20), 5% methanol (V / V), separation voltage -18 kV and gravity sampling 80s × 15.0 cm with a detection wavelength of 225 nm. × 62.0 cm quartz capillary, effective length 50.0 cm. The effect of phosphate concentration, organic modifier, SDS concentration, separation voltage and injection time on the DMP, DEP and DBP enrichment ability was discussed. Under the optimal conditions, the linearity was good, with the correlation coefficient greater than 0.9986. The linear range of DMP, DEP and DBP were 1.25 ~ 240, 1.04 ~ 200 and 1.56 ~ 200 mg / L respectively with the detection limits of 0.26, 0.26 and 0.39 mg / L. The method was applied to the determination of DMP, DEP and DBP in enteric-coated tablets with recoveries of 93.3% -108% and RSDs ≤ 5.2%. Each sample determination can be completed within 10 min.