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目的建立复方制剂瑞格列奈二甲双胍片中瑞格列奈有关物质的检查方法。方法采用HPLC法测定。色谱柱为Agilent ZORBAX SB-C8柱(150 mm×4.6 mm,5μm);以磷酸盐缓冲溶液(p H=3.2)-乙腈(体积比30∶70)为流动相进行梯度洗脱,流速为1.5 m L·min-1;采用荧光检测器,激发波长为244 nm,发射波长为348 nm。结果瑞格列奈与有关物质A(4-羧甲基-2-乙氧基苯甲酸)、有关物质B(2-(3-乙氧基-4-(乙氧羰基)苯基)乙酸)和有关物质D(2-乙氧基-4-[2-[[(1S)-3-甲基-1-[2-(哌啶-1-基)苯基]丁基]氨基)-2-氧代乙基)苯甲酸乙酯)均能有效分离,分离度均大于1.5,且盐酸二甲双胍不干扰有关物质的测定。结论该方法适用于该复方制剂中瑞格列奈的有关物质检查。
Objective To establish a method for the determination of repaglinide in the compound repaglinide metformin tablets. The method was determined by HPLC. The column was an Agilent ZORBAX SB-C8 column (150 mm × 4.6 mm, 5 μm). The gradient elution was performed with a phosphate buffer (p H = 3.2) -acetonitrile (30:70 by volume) m L · min-1. The fluorescence detector was used. The excitation wavelength was 244 nm and the emission wavelength was 348 nm. RESULTS: Repaglinide was associated with substance A (4-carboxymethyl-2-ethoxybenzoic acid), substance B (2- (3-ethoxy- 4- (ethoxycarbonyl) phenyl) And related substance D (2-ethoxy-4- [2 - [[(1S) -3-methyl- 1- [2- (piperidin- 1 -yl) phenyl] butyl] amino) -2 - oxoethyl) benzoate) can be effectively separated, the separation degree is greater than 1.5, and metformin hydrochloride does not interfere with the determination of related substances. Conclusion This method is suitable for the related substances of repaglinide in this compound preparation.