高效液相色谱-质谱联用法测定消癌平片中通关藤苷A、H、I含量  

HPLC-MS Method in Appilication of Determination for Tenacissoside A, H and I Contents in Xiaoaiping Tablets

作　　者：王祁民 孟璐 王小楠 付冉 丁琮洋 郭彩会[1] 孙利民 许剑峰[2] WANG Qi-min;MENG Lu;WANG Xiao-nan;FU Ran;DINGCong-yang;GUO Cai-hui;SUN Li-min;XU Jian-feng(Department of Pharmacy, Hebei People's Hospital of Hebei Province, Shijiazhuang 050051, China;Department of Medical Quality Management, 980 Hospital of PLA Joint Logistic Support Forces, Shijiazhuang 050082, China)

机构地区：[1]河北省人民医院药学部,石家庄050051 [2]解放军联勤保障部队第九八〇(白求恩国际和平)医院质量管理科,石家庄050082

出　　处：《解放军医药杂志》2019年第7期105-108,共4页Medical & Pharmaceutical Journal of Chinese People’s Liberation Army

基　　金：河北省中医药管理局中医药类科研课题计划(冀中医药[2017]67号-2018073);河北省医学科学研究研究重点课题计划(20180176)

摘　　要：目的 建立超高效液相色谱-质谱联用法(UPLC-MS/MS)测定消癌平片中的通关藤苷A、H和I的含量。方法 采用Phenomenex KinetexXB-C18色谱柱,以0.1%甲酸∶乙腈为流动相,线性梯度洗脱,通过电喷雾离子源,多反应监测(MRM),正离子模式。结果 通关藤苷A、H、I质量浓度线性范围分别为0.1~10.0ng/ml(R=0.9997)、0.025~10.0ng/ml(R=0.9995)、0.025~10.0ng/ml(R=0.9989);平均加样回收率分别为97.71%、98.93%和98.92%,RSD分别为1.70%、0.58%和0.49%。消癌平片中通关藤苷A、H、I含量分别为620.33~622.00、310.67~311.33、377.33~379.33μg/g。结论 UPLC-MS/MS方法快速、准确、灵敏,可用于消癌平片中通关藤苷A、H、I的含量测定。Objective To establish high performance liquid chromatography-mass spectrometry (HPLC-MS) method in order to detect Tenacissoside A, H and I contents in Xiaoaiping Tablets. Methods Chromatographic separation was performed on a Phenomenex Kinetex XB-C18 column by a gradient elution, and the mobile phase was composed of acetonitrile and -0.1% formic acid aqueous solution. The MS analysis was performed by multiple reaction monitoring (MRM) via electrospray ionization source (ESI) in positive ion mode. Results Mass concentration of Tenacissoside A, H and I were linear in the range of 0.1-10.0 ng/ml ( R =0.9 997), 0.025-10.00 ng/ml ( R =0.9 995) and 0.025-10.0 ng/ml ( R =0.9 989) respectively, and average recoveries were 97.71%, 98.93% and 98.92% respectively, and relative standard deviation (RSD) values were1.70%, 0.58% and 0.49% respectively. Content ranges of Tenacissoside A, H and I contents in Xiaoaiping Tablets were 620.33-622.00 μg/g,310.67-311.33 μg/g and 377.33-379.33 μg/g respectively. Conclusion High performance liquid chromatography-mass spectrometry method is rapid, accurate and sensitive, and therefore it may be used for content determination of Tenacissoside A, H and I contents in Xiaoaiping Tablets.

关 键 词：消癌平片 超高效液相色谱-质谱联用 通关藤苷A 通关藤苷H 通关藤苷I 

分 类 号：R917[医药卫生—药物分析学]