基于UPLC-Q/TOF-MS分析江西特色炮制工艺对枳壳化学成分的影响  

Analysis of Influence of Jiangxi Characteristic Processing Technology on Chemical Compositions of Aurantii Fructus Based on UPLC-Q/TOF-MS

作　　者：祝婧[1] 袁恩[1] 牟俊雍 钟凌云[1] 张金莲[1] 杨明[1] 刘海平 ZHU Jing;YUAN En;MOU Jun-yong;ZHONG Ling-yun;ZHANG Jin-lian;YANG Ming;LIU Hai-ping(Jiangxi University of Traditional Chinese Medicine;Guilin Medical University,Guilin 541004,China)

机构地区：[1]江西中医药大学,南昌330004 [2]桂林医学院,广西桂林541004

出　　处：《中国实验方剂学杂志》2020年第16期142-153,共12页Chinese Journal of Experimental Traditional Medical Formulae

基　　金：国家重点研发计划项目(2018YFC1707206);国家中医药管理局公益性行业科研专项(201507002-2);江西省自然科学基金项目(20192BAB215055);江西省卫生健康委员会科技计划项目(20195646);江西中医药大学中药学一流学科专项科研基金项目(JXSYLXK-ZHYAO041);江西中医药大学博士科研启动基金课题(2019WBZR007)。

摘　　要：目的:比较不同特色炮制工艺对枳壳化学成分的影响,筛选优势饮片品种。方法:采用UPLC-Q/TOF-MS检测枳壳中化学成分,选择ACQUITY UPLC BEH C18色谱柱(2. 1 mm×100 mm,1. 7μm),流动相0. 1%甲酸水溶液(A)-0. 1%甲酸乙腈溶液(B)梯度洗脱(0~10 min,5%~35%B;10~18 min,35%~75%B;18~21 min,75%~100%B;21~24 min,100%B;24~24. 1 min,100%~5%B;24. 1~28 min,5%B),电喷雾离子源(ESI),正离子模式,质谱扫描范围m/z 50~1 200,通过对照品、相对分子质量、质谱裂解规律和文献信息鉴定枳壳甲醇提取液的化学成分。利用SIMCA-P 13. 0软件建立枳壳各炮制品主成分分析(PCA)模型和偏最小二乘法-判别分析(PLS-DA)模型,获取PCA得分图,PLS-DA载荷图和变量重要性投影(VIP)值,筛选造成枳壳炮制前后主要差异的物质基础。结果:鉴定出了54个化学成分,PCA提示经不同方法炮制后枳壳组间差异性较大,PLS-DA筛选出VIP值>1的14个化学成分作为炮制前后差异性的主要化学标记物,包括橙皮素、枸橘苷、柚皮芸香苷、柚皮苷、橙皮苷、新橙皮苷、橙皮内酯、柚皮素、去乙酰诺米林、去甲川陈皮素、橙皮素5-O-葡萄糖苷、橙皮素7-O-葡萄糖苷、新北美圣草苷和4’,5’-二氢补骨脂素;将其综合加权评分后发现蜜麸枳壳中有效成分含量最高。结论:枳壳炮制前后化学成分含量发生显著变化,黄酮类成分是区分枳壳不同炮制品最重要的化合物类别,江西樟帮蜜麸枳壳为枳壳的优势炮制品种。Objective: To compare the effects of different processing techniques on the chemical constituents of Aurantii Fructus for screening the dominant decoction pieces. Method: UPLC-Q/TOF-MS was used to detect the chemical constituents of Aurantii Fructus,chromatography separation was achieved on an ACQUITY UPLC BEH C18 column(2. 1 mm×100 mm,1. 7 μm),and gradient elution was performed with0. 1% formic acid aqueous solution(A)-0. 1% formic acid acetonitrile solution(B)as mobile phase(0-10 min,5%-35%B;10-18 min,35%-75%B;18-21 min,75%-100%B;21-24 min,100%B;24-24. 1 min,100%-5%B;24. 1-28 min,5%B). Data acquisition was carried out in electrospray ionization(ESI)under the positive ion mode,the scanning range was m/z 50-1 200. The chemical constituents in methanol extract of Aurantii Fructus were identified according to reference substance, relative molecular weight, mass spectrometric cleavage rule and literature information. SIMCA-P 13. 0 software was used to establish principal component analysis(PCA)model and partial least squares-discriminant analysis(PLS-DA)model of Aurantii Fructus processed products,PCA score plot,PLS-DA loading plot and variable importance in the protection(VIP)values were obtained to screen the material basis for the main differences before and after processing of Aurantii Fructus. Result: A total of 54 chemical components were identified by UPLC-Q/TOF-MS. PCA indicated that there were significant differences among different groups of Aurantii Fructus processed by different methods. A total of 14 chemical components with VIP value >1 were screened by PLS-DA as the main chemical markers for the differences before and after processing,including hesperidin,poncirin,narirutin,etc. The comprehensive weighted score showed that the content of effective components in Aurantii Fructus processed with honey bran was the highest. Conclusion: The contents of chemical constituents in Aurantii Fructus before and after processing are significantly changed. Flavonoids are the most important compounds to distinguis

关 键 词：枳壳 炮制 饮片 化学成分 超高效液相色谱-四极杆-飞行时间串联质谱(UPLC-Q/TOF-MS) 主成分分析 偏最小二乘法-判别分析 

分 类 号：R22[医药卫生—中医基础理论] R28[医药卫生—中医学]