目的: 建立HPLC法同时测定小儿肺热咳喘口服液中10个成分(盐酸麻黄碱、盐酸伪麻黄碱、苦杏仁苷、(R,S)-告依春、芒果苷、黄芩苷、连翘苷、绿原酸、连翘酯苷A、木犀草苷) 的含量,为小儿肺热咳喘口服液质量标准完善提供依据。方法: 采用 ZORBAX SB-C18色谱柱(4.6 mm×250 mm,5 μm),流动相为乙腈-0.1%磷酸水溶液,梯度洗脱,体积流量为0.8 mL·min-1,柱温为35 ℃,检测波长为210 nm(盐酸麻黄碱、盐酸伪麻黄碱和苦杏仁苷)、258 nm[(R,S)-告依春、芒果苷、黄芩苷和连翘苷]和330 nm(绿原酸、连翘酯苷A和木犀草苷)。结果: 上述10个成分进样量的线性关系分别为0.20～1.20 μg(r=0.999 0)、0.20～1.20 μg(r=0.999 6)、0.25～1.50 μg(r=0.999 4)、0.40～2.40 μg(r=0.999 5)、0.40～2.40 μg(r=0.999 2)、0.40～2.40 μg(r=0.999 1)、0.40～2.40 μg(r=0.999 3)、0.20～1.20 μg(r=0.999 3)、0.10～0.60 μg(r=0.999 4)、0.50～3.00 μg(r=0.999 6),平均加样回收率为98.5%～99.5%,RSD≤0.89%(n＝9)。单因素方差分析结果表明,不同批次间的盐酸麻黄碱、盐酸伪麻黄碱、苦杏仁苷、黄芩苷、连翘苷、连翘酯苷A、芒果苷含量无显著性差异(P>0.01),(R,S)-告依春、绿原酸和木犀草苷的含量有显著差异(P<0.01)。盐酸麻黄碱、盐酸伪麻黄碱、苦杏仁苷、(R,S)-告依春、绿原酸、木犀草苷、黄芩苷、连翘苷、连翘酯苷A、芒果苷的平均含量分别为0.174、0.067、2.326、3.548、2.851、0.958、3.484、3.456、5.389、3.891 mg·mL-1。结论: 该方法简便、准确、灵敏,重复性好,可用于同时测定小儿肺热咳喘口服液中10个成分的含量。
Objective: To develop an HPLC method for simultaneous determination of ten constituents [ephedrine hydrochloride, pseudoephedrine hydrochloride, amygdalim,(R,S)epigoitrin, mangiferin, baicalin, phillyrin, chlorogenic acid, forsythiaside A and cynaroside] in Xiaoer Feire Kechuan oral solution, so as to offer basis for improvement of the drug's standard. Methods: The analysis was performed on a ZORBAX SB-C18 column (4.6 mm×250 mm, 5 μm) with acetonitrile-0.1% phosphoric acid aqueous solution as mobile phases in gradient elution, 0.8 mL·min-1 as flow rate and 35 ℃ as column temperature. The detection wavelengths were at 210 nm for ephedrine hydrochloride, pseudoephedrine hydrochloride and amygdalim, 258 nm for (R,S) epigoitrin, mangiferin, baicalin and phillyrin and 330 nm for chlorogenic acid, forsythiaside A and cymaroside, respectively. Results: The linear ranges were 0.20-1.20μg(r=0.999 0) for ephedrine hydrochlorid, 0.20-1.20 μg (r=0.999 6) for pseudoephedrine hydrochloride, 0.25-1.50 μg(r=0.999 4) for amygdalim, 0.40-2.40 μg(r=0.999 5) for (R,S)-epigoitrin, 0.40-2.40 μg (r=0.999 2) for chlorogenic acid, 0.40-2.40 μg (r=0.999 1) for cymaroside, 0.40-2.40 μg(r=0.999 3) for baicalin, 0.20-1.20 μg(r=0.999 3) for phillyrin, 0.10-0.60 μg(r=0.999 4) for forsythiaside A and 0.50-3.00 μg (r=0.999 6) for mangiferin, respectively. The average recovery rates were in the range of 98.5%-99.5% with RSDs≤0.89%(n＝9). The results of one-factor analysis of variance showed that there was no significant difference in the contents of ephedrine hydrochloride, pseudoephedrine hydrochloride, amygdalim, baicalin, phillyrin, forsythiaside A and mangiferin, but there was significant difference in the content of (R,S)-epigoitrin, chlorogenic acid and cynaroside between different batches. The average contents of ephedrine hydrochloride, pseudoephedrine hydrochloride,amygdalim, (R,S)-epigoitrin, chlorogenic acid, cynaroside, baicalin, phillyrin, forsythiaside A and mangiferin were 0.174, 0.067, 2.326, 3.548, 2.851, 0.958, 3.484, 3.456, 5.389, 3.891 mg·mL-1, respectively.Conclusion: The developed method is simple, accurate, specific and reproducible, which can be used for determining the contents of ten constituents in Xiaoer Feire Kechuan oral solution.
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