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目的:通过LC-MS法测定抗癌中药复方(仙鹤草、败酱草、龙葵)中9种化学成分,对其水提物和醇提物中各主要成分的含量进行对比,测定灌肠方中抗肿瘤有效成分,为复方制剂有效成分测定提供初步依据。方法:色谱柱为Agilent Zorbax SB-C18柱,流动相为乙腈-0.1%甲酸,梯度洗脱。采用内标法测定各成分的含量,选择离子监测(SIR)模式同时监测复方中的9种成分和2个内标成分;ESI源,正、负离子同时检测。利用所建立的方法对不同提取批次的水提物(3批)和醇提物(3批)进行含量测定。结果:9种化学成分的浓度和峰面积在测定浓度范围内具有良好的线性关系,除儿茶素和鞣花酸外,醇提物中各有效成分的含量均比水提物中的含量高。结论:该方法简便、专属性好、灵敏度高,适用于复方提取液的有效含量测定;复方醇提物优于水提物。复方制剂的有效成分是由单味中药的有效成分协同作用的结果。
OBJECTIVE: To determine the contents of nine main constituents in aqueous extracts and alcohol extracts of nine anti-cancer compounds (Agrimony, Patrinia, Solanum nigrum) by LC-MS method. In the anti-tumor active ingredients, the active ingredient for the preparation of compounds provide a preliminary basis. Methods: The Agilent Zorbax SB-C18 column was used with a mobile phase of acetonitrile-0.1% formic acid, gradient elution. The content of each component was determined by internal standard method. Nine components and two internal standard components in compound prescription were monitored by SIR mode. ESI source, positive and negative ions were simultaneously detected. The established method was used to determine the contents of water extracts (3 batches) and alcohol extracts (3 batches) from different batches. Results: There was a good linear relationship between the concentration and the peak area of the nine chemical constituents in the range of concentration. Except catechin and ellagic acid, the content of each active ingredient in the alcohol extract was higher than that in the water extract . Conclusion: The method is simple, specific and sensitive, suitable for the determination of the effective content of compound extract; compound alcohol extract is better than water extract. The active ingredients of compound preparations are the result of the synergistic effect of the active ingredients of single Chinese medicines.