RP-HPLC法检测甜梦口服液(甜梦合剂)中淫羊藿苷、紫丁香苷和23-乙酰泽泻醇B的含量

Establishment of RP-HPLC method for simultaneous determination of icariin,syringin and 23-acetyl alismatol B in Tianmeng oral liquid(Tianmeng mixture)

目的建立同时检测甜梦口服液(甜梦合剂)中的淫羊藿苷、紫丁香苷和23-乙酰泽泻醇B含量的RP-HPLC法。方法利用Shimadzu CLC ODS C 18(4.6 mm×250 mm,5μm)分离甜梦口服液中3种成分(淫羊藿苷、紫丁香苷和23-乙酰泽泻醇B)。测定波长:淫羊藿苷为271 nm、紫丁香苷为265 nm和23-乙酰泽泻醇B为207 nm;柱温30℃,进样体积10μl。流动相:0.3%磷酸溶液(流动相A)-乙腈(流动相B),洗脱程序:0~4 min(95%A)、4~7 min(95%~78%A)、7~10 min(78%~38%A)、10~16 min(38%~26%A)、16~23 min(26%~19%A)、23~28 min(19%A)、28~28.5 min(19%~95%A)。外标法检测3种成分的含量。结果紫丁香苷、23-乙酰泽泻醇B和淫羊藿苷分别在0.1962~19.62μg/ml,0.7544~75.44μg/ml和0.1966~19.66μg/ml质量浓度范围内存在良好的线性关系,线性系数R 2均大于0.995;平均加标回收率分别为99.47%,98.68%和100.26%;仪器精密度和方法重复性RSD(n=6)均在5.0%以内。结论建立的RP-HPLC法具有线性范围广、检测结果准确等优点,可以用于甜梦口服液(甜梦合剂)供试品的质量控制。

Objective To establish an RP-HPLC analytical method for simultaneous determination of icariin,syringin and 23-acetylzealismol B in Tianmeng oral liquid(Tianmeng mixture).Methods Icariin,syringin and 23-acetylzealismol B were isolated from Tianmeng oral liquid on Shimadzu CLC ODS C 18(4.6 mm×250 mm,5μm).The determination wavelength was 271 nm for icariin,265 nm for syringin and 207 nm for 23-acetylzelatol B.The column temperature was 30℃and the sample injection volume was 10μl.The 0.3%phosphoric acid solution(A)-acetonitrile(B)was used as the mobile phase.The gradient elution procedure was as follows:0-4 min(95%A),4-7 min(95%-78%A),7-10 min(78%-38%A),10-16 min(38%-26%A),16-23 min(26%-19%A),23-28 min(19%A),28-28.5 min(19%-95%A).The contents of three components were detected by RP-HPLC external standard method.Results Syringin,23-acetylzelatol B and icariin showed good linear relationships in the concentration ranges of 0.1962-19.62μg/ml,0.7544-75.44μg/ml and 0.1966-19.66μg/ml,and all correlation coefficients(R 2)were above 0.995.The average recoveries were 99.47%,98.68%and 100.26%,respectively,with RSD of precision and repeatability less than 5.0%(n=6).Conclusion This established RP-HPLC method has advantages of wide linear range and high accuracy,which is suitable for the quality control of Tianmeng oral liquid(Tianmeng mixture).