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目的:建立RP-HPLC法测定氯磺丙脲有关物质。方法:采用Waters2695型高效液相色谱仪,色谱柱为KromasilC18(4.6mm×250mm,5μm)色谱柱,流动相为乙腈-磷酸二氢铵溶液(取磷酸二氢铵1.725g,加水300mL使溶解,用磷酸调节pH至3.50±0.05)(625∶375),流速1.0mL.min-1,检测波长200nm。结果:氯磺丙脲与其相关杂质分离度良好,浓度在0.15～7.5μg·mL-1范围内与峰面积呈良好的线性关系(r=0.9999,n=6);已知杂质4-氯苯磺酰胺的相对响应因子为0.86,1,3-二丙基脲的相对响应因子为3.9;氯磺丙脲最低检出量为3ng。结论:本方法专属性好,灵敏度高,结果准确,可用于氯磺丙脲质量控制。
Objective: To establish a RP-HPLC method for the determination of chlorpropamide-related substances. METHODS: Waters 2695 high performance liquid chromatograph was used. The column was Kromasil C18 (4.6 mm × 250 mm, 5 μm). The mobile phase consisted of acetonitrile-ammonium dihydrogen phosphate solution (1.725 g ammonium dihydrogen phosphate and 300 mL water) The pH was adjusted to 3.50 ± 0.05 with phosphoric acid (625: 375) at a flow rate of 1.0 mL.min-1 with a detection wavelength of 200 nm. Results: The separation of chlorpropamide and its related impurities was good, with a good linear relationship (r = 0.9999, n = 6) with the peak area in the range of 0.15 ~ 7.5μg · mL-1. The relative response factor for sulfonamide was 0.86, and the relative response factor for 1,3-dipropyl urea was 3.9. The lowest detection limit for chlorpropamide was 3 ng. Conclusion: The method has good specificity, high sensitivity and accurate results, which can be used for the quality control of chlorpropamide.