目的 建立复方布洛肾素那敏片有关物质检查的方法。方法 采用Ultimate C₁₈色谱柱(4.6 mm×250 mm, 5 μm);磷酸溶液(pH 2.5)-乙腈为流动相, 1.0 mL·min^-1的流速梯度洗脱, 在214 nm处检查本品中布洛芬(IBU)的有关物质;以乙腈-0.1%辛烷磺酸钠溶液(磷酸调pH至3.0)(20∶80)为流动相A, 乙腈-磷酸盐缓冲液(1.15%磷酸二氢铵, 0.1%辛烷磺酸钠, 磷酸调pH至3.0)(60∶40)为流动相B, 1.5 mL·min^-1的流速梯度洗脱, 在215 nm处检查本品中去氧肾上腺素(PE)和氯苯那敏(CHL)的有关物质。结果 主成分与已知杂质以及各杂质之间分离良好、专属性强, 布洛芬、布洛芬毒性杂质C、去氧肾上腺素及氯苯那敏的检测限分别为50.5、42.9、52.5和47.4 ng·mL^-1。结论 所建立的方法可用于本品的有关物质检查。

OBJECTIVE To establish a HPLC method for the detection of related substances of allergy and congestion relief. METHODS An Ultimate C₁₈ column(4.6 mm×250 mm, 5 μm)was used. Gradient elution was used to determine the related substances of ibuprofen with phosphoric acid solution(pH 2.5)as mobile phase A and acetonitrile as mobile phase B. The flow rate was 1.0 mL·min^-1 and the detection wavelength was set at 214 nm. As for the related substances of phenylephrine and chlorphenamine, gradient elution was used with acetonitrile-0.1% octanesulfonic acid sodium(pH was adjusted to 3.0 with phosphoric acid)(20∶80)as mobile phase A and acetonitrile-phosphate buffer(1.15% ammonium dihydrogen phosphate, 0.1% octanesulfonic acid sodium, pH adjusted to 3.0 with phosphoric acid)(60∶40)as mobile phase B. The flow rate was 1.5 mL·min^-1, and the detection wavelength was set at 215 nm. RESULTS The related substances were completely separated from the principal components. The detection limits were 50.5, 42.9, 52.5 and 47.4 ng·mL^-1 for ibuprofen, ibuprofen′s impurity C, phenylephrine, and chlorphenamine, respectively. CONCLUSION The method is suitable for detection of the related substances in allergy and congestion relief.