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目的:建立同时测定甲基多巴含量及有关物质的HPLC方法。方法:采用反相高效液相色谱法,色谱柱为Venusil XBPC18(4.6mm×250mm,5μm)柱,以甲醇-0.1mol·L-1磷酸溶液(用稀氨水调节pH至3.0)为流动相进行梯度洗脱(0～8min,10∶90;8～20min,10∶90→75∶25;20～25min,75∶25;25～26min,75∶25→10∶90;26～35min,10∶90),柱温35℃,流速1.0mL.min-1,检测波长280nm。结果:甲基多巴峰与各主要杂质及强制破坏产生的降解产物的杂质峰均分离良好,甲基多巴浓度在21.60～194.4μg·mL-1范围内,与峰面积呈良好的线性关系,回归方程A=1.338×104C-5.369×103,r=1.0000(n=7);重复性试验RSD为0.41%(n=6);平均加样回收率为99.9%(RSD=0.48%,n=9);最低检测限为2.084ng;供试品溶液在24h内稳定。结论:本方法准确、灵敏、可靠,专属性强,可用于甲基多巴的质量控制。
Objective: To establish a HPLC method for simultaneous determination of methyldopa and related substances. Methods: Reversed-phase high performance liquid chromatography (RP-HPLC) was performed on a Venusil XBPC18 column (4.6 mm × 250 mm, 5 μm) using methanol-0.1 mol·L-1 phosphoric acid solution Gradient elution (0-8 min, 10:90; 8-20 min, 10:90 → 75:25; 20-25 min, 75:25; 25-26 min, 75:25 → 10:90; 26-35 min, 10: 90), column temperature 35 ℃, flow rate 1.0mL.min-1, detection wavelength 280nm. Results: The peaks of methyldopa were separated from the major impurities and the impurity peaks of the degradation products. The concentration of methyldopa was in the range of 21.60-194.4 μg · mL-1, and showed a good linear relationship with the peak area , The regression equation A = 1.338 × 104C-5.369 × 103, r = 1.0000 (n = 7); the repeatability test RSD was 0.41% (n = 6); the average recovery was 99.9% (RSD = 0.48%, n = 9); The minimum detection limit is 2.084ng; The test solution is stable within 24h. Conclusion: The method is accurate, sensitive, reliable and specific. It can be used for the quality control of methyldopa.