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目的:建立沙美特罗替卡松粉吸入剂有关物质的HPLC测定方法。方法:采用Phenomenex Luna C18色谱柱(4.6 mm×250 mm,5μm);以0.05%磷酸溶液-甲醇(97∶3)为流动相A,0.05%磷酸乙腈溶液-甲醇(97∶3)为流动相B,进行梯度洗脱,流速1 mL.min-1;检测波长228 nm;柱温40℃。结果:沙美特罗替卡松主要成分峰与其相关物质峰完全分离,沙美特罗和丙酸氟替卡松浓度分别在0.045～4.5μg.mL-1和0.01～10.14μg.mL-1范围内呈良好线性关系,最低检测限(S/N≥3)分别为4 ng和1 ng。结论:该方法专属性好,精密度、稳定性符合要求,方法可靠,可用于沙美特罗替卡松粉吸入剂有关物质的测定。
OBJECTIVE: To establish a HPLC method for the determination of related substances of salmeterol powder inhalation. METHODS: Phenomenex Luna C18 column (4.6 mm × 250 mm, 5 μm) was used. The mobile phase consisted of 0.05% phosphoric acid solution-methanol (97: 3) as mobile phase A and 0.05% B, gradient elution, flow rate 1 mL.min-1; detection wavelength 228 nm; column temperature 40 ℃. Results: The major component peaks of salmeterol and ticalaprexacin were completely separated from the related substance peaks. The concentrations of salmeterol and fluticasone propionate were linear in the range of 0.045-4.5μg.mL-1 and 0.01-10.1μg.mL-1, respectively Relationship, the minimum detection limit (S / N ≥ 3) were 4 ng and 1 ng. Conclusion: The method is of good specificity, precision and stability to meet the requirements. The method is reliable and can be used for the determination of related substances in salmeterol powder.