目的: 采用HPLC法同时测定盐酸赛洛唑啉鼻用喷雾剂中盐酸赛洛唑啉、羟苯甲酯和羟苯丙酯的含量,并进行递送剂量均一性和有关物质检查。方法: 采用SHISEIDO CAPCELL PEK C18色谱柱(250 mm×4.6 mm,5 μm),以乙腈-0.1%三乙胺(用冰醋酸调节pH至5.0)(45∶55)为流动相,流速1.0 mL·min-1,检测波长220 nm,柱温30 ℃,进样量10 μL。结果: 盐酸赛洛唑啉、羟苯甲酯和羟苯丙酯质量浓度分别在5.360~107.2 μg·mL-1(r=1.000),2.124~42.48 μg·mL-1(r=0.999 9),1.034~20.68 μg·mL-1(r=1.000)范围内具有良好的线性关系。盐酸赛洛唑啉、羟苯甲酯和羟苯丙酯的平均回收率(n=9)分别为102.2%、101.4%、101.5%。3批样品中盐酸赛洛唑啉的含量分别为101.0%、101.1%、100.5%;羟苯甲酯的含量分别为0.22、0.21、0.21 mg·mL-1;羟苯丙酯的含量分别为0.10、0.10、0.10 mg·mL-1。递送剂量均一性10个结果均在平均值的75%~125%。杂质Ⅰ的含量分别为1.6%、1.8%、1.9%。结论: 经方法学验证,该方法简便、高效、准确,重复性好,可应用于盐酸赛洛唑啉鼻用喷雾剂的质量控制和标准研究。
Objective: To establish an HPLC method for determination of the content of xylometazoline hydrochloride, methylparaben and propylparaben, the uniformity of delivery dose and related substance in xylometazoline hydrochloride nasal spray. Methods: SHISEIDO CAPCELL PEK C18(250 mm×4.6 mm, 5 μm)was adopted with the mobile phase of acetonitrile-0.1% triethylamine (the pH was adjusted to 5.0 with acetic acid) (45∶55) at the flow rate of 1.0 mL·min-1. The detection wavelength was 220 nm. The column temperature was 30 ℃.The injection volume was 10 μL. Results: The calibration curves of xylometazoline hydrochloride, methylparaben and propylparaben were in good linear relation in the ranges of 5.360-107.2 μg·mL-1(r=1.000), 2.124-42.48 μg·mL-1(r=0.999 9), 1.034-20.68 μg·mL-1(r=1.000), respectively. The average recoveries of xylometazoline hydrochloride, methylparaben and propylparaben were 102.2%, 101.4%, 101.5%. In the three batches of samples, the content of xylometazoline hydrochloride was 101.0%, 101.1%, 100.5%, the content of methylparaben was 0.22, 0.21, 0.21 mg·mL-1,and propylparaben was 0.10, 0.10, 0.10 mg·mL-1, respectively. The ten results of the uniformity of delivery dose were between 75%-125%. The content of impurity I was 1.6%, 1.8%, 1.9%, respectively. Conclusion: The method is simple, rapid, accurate, and reproducible. It can offer reference for quality control and standard research of the drug.
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