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
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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 Kinetex XB-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0.1～10.0 ng/ml(R=0.9 997)、0.025～10.0 ng/ml(R=0.9 995)、0.025～10.0 ng/ml(R=0.9 989);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 were 1.70%, 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.
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 were 1.70%, 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.
引文
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[13] 伍锡栋,姚闵,李玉云,等.乌骨藤苷晶体对人宫颈腺癌荷瘤裸鼠肿瘤抑制作用的实验研究[J].实验动物科学,2014,31(6):7-10.
[14] 邹渭洪,付成效,邓丽菁.乌骨藤总苷抑制肝癌细胞增殖和AFP分泌[J].中南医学科学杂志,2013,41(4):344-346.
[15] 常伟,李培培,袁平凡,等.乌骨藤总皂苷对对乙酰氨基酚诱导的小鼠肝损伤的保护作用[J].中国新药杂志,2015,24(24):2835-2838,2853.
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[2] 吴建钟,袁治顺,于良.消癌平联合5-氟尿嘧啶处理对肝癌细胞体外生长及癌基因表达的影响[J].海南医学院学报,2017,23(6):728-731,735.
[3] 武阳.伊立替康单药与联合消癌平治疗老年晚期胃癌的比较研究[J].中国药房,2016,27(5):657-659.
[4] 程蒙蒙,佘明金,荣辉,等.消癌平注射液联合同步放化疗治疗食管癌的临床观察[J].中国临床医生杂志,2018,46(10):1207-1211.
[5] 国家食品药品监督管理局.WS3-B-3959-98-2013消癌平片[S].2014-01-08.
[6] 韩丽,张慧,康廷国,等.中药通关藤的研究进展[J].中华中医药学刊,2016,34(10):2329-2331.
[7] 白爽,李奕诺,徐鑫,等.通关藤化学成分及药理活性研究进展[J].解放军药学学报,2015,31(3):260-264.
[8] 徐佳佳,陆兔林,王云峰,等.不同产地通关藤饮片中绿原酸及总酚酸的含量比较[J].中国药业,2008,17(23):21-23.
[9] 刘峰群,曹红,靳守东,等.通关藤注射液酚酸类成分指纹图谱的HPLC测定[J].中成药,2003,25(3):175-178.
[10] 潘成学,刘伟,申小静.高效液相色谱法测定消癌平片中绿原酸的含量[J].中国药业,2005,14(8):26-27.
[11] 方奕奇,孙雪梅.通关藤化学成分及抗肿瘤作用的研究进展[J].中国生化药物杂志,2011,32(2):165-167.
[12] 林耀才.乌骨藤总苷对SGC-7901、S_(180)、P_(388)肿瘤细胞的抑制作用研究[J].药学研究,2015,34(7):376-378,383.
[13] 伍锡栋,姚闵,李玉云,等.乌骨藤苷晶体对人宫颈腺癌荷瘤裸鼠肿瘤抑制作用的实验研究[J].实验动物科学,2014,31(6):7-10.
[14] 邹渭洪,付成效,邓丽菁.乌骨藤总苷抑制肝癌细胞增殖和AFP分泌[J].中南医学科学杂志,2013,41(4):344-346.
[15] 常伟,李培培,袁平凡,等.乌骨藤总皂苷对对乙酰氨基酚诱导的小鼠肝损伤的保护作用[J].中国新药杂志,2015,24(24):2835-2838,2853.
[16] 张小磊,苏远,方海明,等.乌骨藤总皂苷对四氯化碳诱导的雄性大鼠肝纤维化的保护作用[J].中国新药杂志,2017,26(9):1047-1052.