HPLC法同时测定复方苦参注射液中7个成分含量及指纹图谱研究  

Determination of seven components in compound Kushen injection by HPLC and fingerprint study

作　　者：王鹏飞 王京辉[2] 段秀梅 张亚锰 毕小凤 海丽娜 游蓉丽 WANG Peng-fei;WANG Jing-hui;DUAN Xiu-mei;ZHANG Ya-meng;BI Xiao-feng;HAI Li-na;YOU Rong-li(Beijing Zhendong Guangming Pharmaceutical Research Institule Co.,Ltd.,Bejing 100085,China;Beijing Institute for Drug Control,Beijing Key Lab Analysis and Evaluation on Chinese Medicine,Beijing 102206,China)

机构地区：[1]北京振东光明药物研究院有限公司,北京100085 [2]北京市药品检验所中药成分分析与生物评价北京市重点实验室,北京102206

出　　处：《药物分析杂志》2022年第7期1101-1109,共9页Chinese Journal of Pharmaceutical Analysis

基　　金：国家中药标准化建设(ZYBZH-C-JIN-43);国家重点研发计划项目(2017YFC1701900)。

摘　　要：目的:建立HPLC法同时测定复方苦参注射液中7个成分(甲基氧化偶氮甲醇樱草糖苷、苦参碱、槐果碱、槐定碱、氧化槐果碱、氧化苦参碱、番石榴酸)的含量及指纹图谱研究,为其质量控制提供依据。方法:采用Waters Xselect CSH^(TM)C_(18)色谱柱(250 mm×4.6 mm, 5μm),以甲醇-0.2%磷酸二氢钾为流动相,梯度洗脱,流速0.6 mL·min^(-1),柱温30℃,检测波长211 nm。结果:在建立的液相色谱条件下,测定的甲基氧化偶氮甲醇樱草糖苷、苦参碱、槐果碱、槐定碱、氧化槐果碱、氧化苦参碱、番石榴酸7个成分的平均加样回收率分别为95.7%、101.3%、100.8%、101.7%、102.6%、102.5%、99.5%,RSD分别为2.0%、0.72%、0.90%、0.74%、1.4%、0.96%、1.8%;10批次样品中7个成分的含量分别为0.53~0.73、2.66~4.22、0.75~1.11、0.70~0.89、2.20~2.84、7.62~9.95、1.63~2.20 mg·mL^(-1)。在相同液相色谱条件下建立的指纹图谱测定方法确立了9个共有峰,生成对照图谱,10批样品的相似度测定结果在0.99以上。结论:本研究同时对复方苦参注射液的主要成分进行定量分析和指纹图谱进行定性分析,含量测定准确,指纹峰特征性强,该方法稳定可靠,可为复方苦参注射液的质量控制与评价提供参考。Objective:To establish an HPLC method for simultaneous determination of seven components(macrozamin, matrine, sophocarpine, sophoridine, oxysophocarpine, oxymatrine and piscidic acid) in compound Kushen injection and the fingerprint, providing the evidence for the quality control and evaluation of compound Kushen injection. Methods: Waters Xselect CSH^(TM)C_(18)column(250 mm×4.6 mm, 5 μm) was adopted, the mobile phase consisted of methanol-0.2% potassium dihydrogen phosphate with gradient elution. The flow rate was 0.6 mL·min^(-1), the detection wavelength was set at 211 nm and the column temperature was set at 30 ℃. Results: Under the above chromatographic conditions, the average recovery rates of macrozamin, matrine, sophocarpine, sophoridine, oxysophocarpine, oxymatrine and piscidic acid were 95.7%, 101.3%, 100.8%, 101.7%, 102.6%, 102.5% and 99.5% with RSDs of 2.0%, 0.72%, 0.90%, 0.74%, 1.4%, 0.96% and 1.8%, respectively. The contents of 7 components in 10 batches of samples were 0.53-0.73, 2.66-4.22, 0.75-1.11, 0.70-0.89, 2.20-2.84, 7.62-9.95 and 1.63-2.20 mg·mL^(-1), respectively. The HPLC fingerprints of compound Kushen injection were established and 9 peaks were distinguished by developed HPLC method. And the similarities of HPLC fingerprints of 10 different batches were all above 0.99. Conclusion: The established method can perform the quantitative analysis of the main components and the qualitative analysis of the fingerprint simultaneously. The assay method is accurate and the fingerprint peaks are characteristic. The method is stable and reliable, which can provide supporting evidence for quality control and evaluation of CKI.

关 键 词：复方苦参注射液 高效液相色谱 甲基氧化偶氮甲醇樱草糖苷 苦参碱 槐果碱 槐定碱 氧化槐果碱 氧化苦参碱 番石榴酸 指纹图谱 相似度 

分 类 号：R917[医药卫生—药物分析学]