反相高效液相梯度洗脱法测定地松磺胺麻黄碱滴鼻液中有效成分含量

 目的 建立同时测定地松磺胺麻黄碱滴鼻液中有效成分含量的反相高效液相梯度洗脱法（reverse-phase high performance liquid chromatography，RP-HPLC）。方法 采用Agilent Eclipse XDB-C18（250 mm×4.6 mm，5 μm）色谱柱，以甲醇（A）-0.1%磷酸水溶液（B）为流动相进行梯度洗脱，梯度洗脱程序为：进样0~10 min，调节流动相A∶B（30∶70，V/V）；10~18 min，流动相A∶B（70∶30，V/V）；18~20 min，流动相A∶B（30∶70，V/V）；流速：1.0 mL/min，检测波长为梯度波长：0~5 min，220 nm；5~8 min，310 nm；8~20 min，240 nm；柱温：30℃，进样量：10 μL。结果 盐酸麻黄碱、磺胺甲噁唑和醋酸地塞米松分别在0.083~0.667 g /L、0.417~3.333 g/L和0.003~0.027 g/ L范围内与峰面积呈良好的线性关系；相关系数分别为：0.999 7、0.999 8和0.999 5；平均回收率分别为：（100.2±1.6）%时RSD为1.61%，（100.4±1.3）%时RSD为1.29%，（99.8±1.4）%时RSD为1.74%。样品中3者平均含量分别为（97.2±3.1）%时RSD为3.06%，（98.6±1.1）%时RSD为1.13%，以及（97.8±1.2）%时RSD为1.23%。结论 该方法简便、快速、专属性强，可用于地松磺胺麻黄碱滴鼻液的质量控制。

Determination of active constituent in dexamethasone acetate,sulfamethoxazole and ephedrine nasal drops by RP-HPLC gradient elution method

Objective To establish a reverse-phase high performance liquid chromatography (RP-HPLC) gradient elution method for the simultaneous determination of ephedrine, sulfamethoxazole and dexamethasone acetate in nasal drops. Methods The samples were separated on a Agilent Eclipse XDB-C18 (250 mm×4.6 mm, 5 μm) by mobile phase of methanol (A) and 0.1% phosphonic acid solution (B) with gradient elution. The program of gradient elution was as follows: The volume ratio of mobile phase A:B was 30:70 between 0 min and 10 min; the volume ratio of mobile phase A:B was 70:30 between 10 min and 18 min; the volume ratio of mobile phase A:B was 30:70 between 18 min and 20 min. The flow rate was 1.0 mL/min and the program of UV gradient absorbance detection was as follows: 0-5 min, at 220 nm; 5-8 min, at 310 nm; 8-20 min, at 240 nm. The column temperature was 30℃ and the sample volume was 10 μL. Results The linear concentration ranges of the calibration curves for ephedrine, sulfamethoxazole and dexamethasone acetate were 0.083-0.667, 0.417-3.333 and 0.003-0.027 g/L, and the coefficient of correlation for ephedrine, sulfamethoxazole and dexamethasone acetate were 0.999 7 (n=5), 0.999 8 (n=5) and 0.999 5 (n=5), respectively. The average recoveries for ephedrine, sulfamethoxazole and dexamethasone acetate were (100.2±1.6)% with RSD of 1.61%, (100.4±1.3)% with RSD of 1.29%, and (99.8± 1.4)% with RSD of 1.74%, respectively. The average content for ephedrine, sulfamethoxazole and dexamethasone acetate were (97.2±3.1)% with RSD of 3.06%, (98.6±1.1)% with RSD of 1.13%, and (97.8±1.2)% with RSD of 1.23%, respectively. Conclusions The RP-HPLC gradient elution method is rapid, sensitive, precise and specific. It could be used to control the quality of dexamethasone acetate, sulfamethoxazole and ephedrine nasal drops.