LC-MS/MS法测定麻黄-桂枝药对中11个成分及其溶出影响的探讨

Determination of eleven analytes and its dissolution effects in drug pair of Ephedrae Herba and Cinnamomi Ramulus by LC-MS/MS

目的 建立麻黄-桂枝药对中原儿茶酸、儿茶素、表儿茶素、丁香醛、香豆素、肉桂醇、肉桂酸、桂皮醛、麻黄碱、伪麻黄碱和甲基麻黄碱11个成分的液相色谱-串联质谱(LC-MS/MS)含量测定方法,并探讨单煎共煎对11个成分溶出的影响。方法 分别以麻黄桂枝共煎液、单煎液、单煎合并液为样品,采用液相色谱-串联质谱法测定8个苯丙素类成分和3个麻黄类生物碱的含量。结果 11个成分在各自范围内均呈良好的线性关系(r≥0.994 8);平均加样回收率为98.30%~100.92%,RSD≤5.85%(n=9);精密度、重复性和稳定性均良好,符合方法学考察要求。麻黄与桂枝共煎时,8个苯丙素类成分煎出量均有不同程度的降低,而3个麻黄类生物碱均有不同程度升高。结论 该方法简便快速、准确可靠,可用于11个成分的含量测定,共煎对麻黄桂枝各自成分的溶出均具有一定的影响。

Objective To establish a LC-MS/MS method of the determination of protocatechuic acid, catechin, epicatechin, eugenol, coumarin, cinnamyl alcohol, cinnamic acid, cinnamaldehyde, ephedrine, pseudoephedrine and methylephedrine in Ephedrae-Cinnamomi herb pair, and investigated the effects of single-decoction and combined-decoction on dissolution of eleven components.Methods Using the ephedrae-cinnamomi decoction, cinnamomi decoction, ephedrae decoction, ephedrae and cinnamomi combined decoction as the test samples, the eight phenylpropanoid compounds and three ephedra alkaloids were determined by LC-MS/MS.Results The 11 indicative components had good linearity(r≥0.994 8).The average recoveries were 98.30%~100.92%,RSD≤5.85%(n=9).The precision, repeatability and stability are all good, meeting the methodological requirements.When Ephedra and Cinnamomi were decocted together, the amount of eight kinds of phenylpropanoid components decreased in different degrees, while the alkaloids of three kinds of ephedra increased in different degrees.Conclusion This method was simple, rapid, accurate and reliable, can be used for the determination of eleven components.The co-decoction had a certain effect on the dissolution of the components of Ephedra and Cinnamomi.