基于UPLC-Q-TOF-MS^E技术的三勒浆口服液上清液及沉淀部分化学成分分析  

Analysis of Chemical Components in Supernatant and Precipitate of Sanajon Oral Liquid Based on UPLC-Q-TOF-MS^E Technology

作　　者：黄浩洲 仇敏 唐进法[2] 李梦琪 刘海燕 樊三虎 谭鹏 韩丽[1] 林俊芝 张定堃[1] HUANG Hao-zhou;QIU Min;TANG Jin-fa;LI Meng-Qi;LIU Hai-yan;FAN San-hu;TAN Peng;HAN Li;LIN Jun-zhi;ZHANG Ding-kun(School of Pharmacy,State Key Laboratory of Characteristic Chinese Drug Resources in Southwest China,Chengdu University of Traditional Chinese Medicine(TCM),Chengdu 611137,China;The First Affiliated Hospital of Henan University of TCM,Zhengzhou 450000,China;Sichuan Nursing Vocational College,Chengdu 610100,China;Sanajon Pharmaceutical Group,Chengdu 610000,China;State Key Laboratory of Biological Evaluation of TCM Quality,National Administration of TCM,Sichuan Academy of Chinese Medicine Sciences,Chengdu 610041,China;Teaching Hospital of Chengdu University of TCM,Chengdu 610072,China)

机构地区：[1]成都中医药大学药学院,西南特色中药资源国家重点实验室,成都611137 [2]河南中医药大学第一附属医院,郑州450000 [3]四川护理职业学院,成都610100 [4]成都市三勒浆药业集团,成都610000 [5]四川省中医药科学院国家中医药管理局中药质量生物评价重点研究室,成都610041 [6]成都中医药大学附属医院,成都610072

出　　处：《中国实验方剂学杂志》2020年第14期143-151,共9页Chinese Journal of Experimental Traditional Medical Formulae

基　　金：国家自然科学基金面上项目(81973493)。

摘　　要：目的:分析三勒浆口服液上清液和沉淀部分的主要化学成分,为建立其质量标准与沉淀控制技术提供依据。方法:使用UPLC-Q-TOF-MSE技术分别对分离后的上清液及沉淀部分化学成分进行定性分析,采用Waters ACQUITY UPLC BEH C18色谱柱(2.1 mm×100 mm,1.7μm),流动相选择0.1%甲酸水溶液(A)-乙腈(B)梯度洗脱(0~1 min,2%B;1~2 min,2%~5%B;2~4 min,5%~7%B;4~6 min,7%~24%B;6~10 min,24%~42%B;10~12 min,42%~54%B;12~15 min,54%~76%B;15~18 min,76%~100%B),流速0.3 mL·min^-1,柱温30℃,进样量2μL。质谱分析采用电喷雾离子源(ESI),负离子模式下使用时间依赖型MSE方式采集样品质谱数据,采集范围m/z 50~1200(上清液)和m/z 50~3000(沉淀),通过对采集数据的保留时间、精确相对分子质量和二级质谱裂解碎片进行比对后鉴定化学成分。结果:在三勒浆口服液上清液中共鉴定了61个化合物,包括鞣质类、酚酸类、黄酮类、氨基酸类、有机酸类、脂肪酸类等;沉淀中共鉴定了15个化合物,包括鞣质类、酚酸类、黄酮类、脂肪酸类等。结论:三勒浆口服液的水解鞣质可能是该制剂潜在的沉淀物质基础,其沉淀物很可能是以鞣花酸和鞣红为主构成的复杂沉淀。建立的UPLC-Q-TOF-MSE可快速、全面地分析三勒浆口服液的化学成分,可为其物质基础、沉淀机制及质量控制等研究提供科学依据。Objective:To analyze the main chemical components in the supernatant and precipitate of Sanajon oral liquid,so as to provide basis for establishing its quality standard and precipitation control technology.Method:UPLC-Q-TOF-MS^E was used to analyze the chemical components in the supernatant and precipitate of this oral liquid.The analysis was performed on Waters ACQUITY UPLC BEH C18 column(2.1 mm×100 mm,1.7μm)with the mobile phase of 0.1%formic acid solution(A)and acetonitrile(B)for gradient elution(0-1 min,2%B;1-2 min,2%-5%B;2-4 min,5%-7%B;4-6 min,7%-24%B;6-10 min,24%-42%B;10-12 min,42%-54%B;12-15 min,54%-76%B;15-18 min,76%-100%B),the flow rate was set to 0.3 mL·min^-1,the column temperature was 30℃,the injection volume was 2µL.The mass spectrographic analysis was used with electrospray ionization(ESI),sample MS data was acquired by time-dependent MSE in negative ion mode,the collection range was m/z 50-1200(supernatant)and m/z 50-3000(precipitate).Then the chemical constituents were identified by the information of retention time,accurate relative molecular mass and secondary mass spectrum fragment.Result:Totally 61 compounds were identified in the supernatant,including tannins,phenolic acids,flavonoids,amino acids,organic acids,fatty acids,etc.Totally 15 compounds were identified in the precipitate,including tannins,phenolic acids,flavonoids,fatty acids,etc.Conclusion:The hydrolyzed tannin of Sanajon oral liquid may be the potential material basis of its precipitate,and its precipitate is likely to be a complex precipitate mainly composed of ellagic acid and tanned red.The established UPLC-Q-TOF-MS^E can quickly and comprehensively analyze the chemical composition of Sanajon oral liquid,which can provide a scientific basis for the researches of its material basis,precipitation mechanism and quality control.

关 键 词：三勒浆 口服液 沉淀 多酚 鞣质 鞣花酸 鞣红 

分 类 号：R22[医药卫生—中医基础理论] R914[医药卫生—中医学]