基于UPLC-Q-TOF-MS分析白术及其不同炮制品化学成分及其差异  

Analysis of chemical constituents of Atractylodis Macrocephalae Rhizoma and its different processed products based on UPLC/Q-TOF-MS/MS

作　　者：吴晓莹 张安然[1] 杨丹阳 朱盈徽 肖小林 吴静雨 徐万爱 龚千锋[1] 于欢[1] WU Xiao-ying;ZHANG An-ran;YANG Dan-yang;ZHU Ying-hui;XIAO Xiao-lin;WU Jing-yu;XU Wa-nai;GONG Qian-feng;YU Huan(Jiangxi University of Chinese Medicine,Nanchang 330004,China)

机构地区：[1]江西中医药大学,江西南昌330004

出　　处：《时珍国医国药》2023年第10期2395-2403,共9页Lishizhen Medicine and Materia Medica Research

基　　金：国家自然科学基金(82104392,82160749);江西省自然科学基金项目(20212BAB216011)。

摘　　要：目的采用超高效液相色谱-四级杆-飞行时间串联质谱法(UPLC-Q-TOF-MS)对白术生品及其4种炮制品的成分进行快速分析及鉴定,找出炮制前后差异成分。方法运用Titank C18色谱柱(2.1 mm×100 mm,1.8μm),流动相0.1%甲酸水溶液(A)-乙腈(B)梯度洗脱(正离子模式:0~0.01 min,5%B;0.01~5 min,5%~30%B;5~14 min,30%~60%B;14~23min,60%~70%B;23~31 min,70%~95%B;31~35 min,95%B)正离子模式检测,电喷雾离子源(ESI),扫描范围m/z 50~1250。结合对照品、数据库及相关文献对白术及其炮制品进行化学成分鉴定。各样品数据经MarkView 1.2.1归一化处理后导入SIMCA 14.1中进行主成分分析(PCA)及偏最小二乘法-判别分析(PLS-DA),通过变量重要性投影(VIP)值>1且t检验中P<0.01的原则,筛选得到白术炮制前后差异成分。结果共鉴定出57个化学成分,白术50个成分,麸炒白术53个成分,土炒白术48个成分,焦白术46个成分,漂白术48个成分。经PCA及PLS-DA发现白术及其不同炮制品的成分具有明显的差异,共筛选出白术内酯Ⅰ、白术内酯Ⅱ、白术内酯Ⅲ及双白术内酯等23个炮制差异成分。结论白术中主要含有萜类、有机酸类及聚乙炔类成分,其中白术内酯Ⅰ、Ⅱ、Ⅲ等有效成分炮制后含量增加,可为白术炮制物质基础研究提供参考。Objective To quickly analyze and identify the components in raw and 4 kinds of processed products of Atractylodis Macrocephalae Rhizoma by ultra-high performance liquid chromatography-quadrupole-time-of-flight mass spectrometry(UPLC-Q-TOF-MS),and then find out the differential components before and after processing.Methods The Titank C18 column(2.1 mm×100 mm,1.8μm)was used with 0.1%formic acid aqueous solution(A)-acetonitrile(B)gradient elu-tion(Positive ion mode:0~0.01 min,5%B;0.01~5 min,5%~30%B;5~14 min,30%~60%B;14-23 min,60%~70%B;23~31 min,70%~95%B;31~35 min,95%B)Electrospray ionization was selected for collection and detection in positive ion with a scan range of m/z 100~1250.Combining the reference substance,chemical databases and related literature information,PeakView1.2 software was used to identify the chemical components of Atractylodis Macrocephalae Rhizoma and its processed products.After normalized treatment by MarkView 1.2.1,the MS data of each sample were analyzed with principal component a-nalysis(PCA)and partial least squares discriminant analysis(PLS-DA)in SICMA 14.1 software,and then the differential com-ponents before and after processing were screened according to the principle of variable importance projection(VIP)value>1 and P<0.01 in t-test.Results A total of 57 components were identified from Atractylodis Macrocephalae Rhizoma and its pro-cessed products,including 50 components of Atractylodis Macrocephalae Rhizoma,53 components of bran-fried Atractylodis Macrocephalae Rhizoma,48 components of stir-baked Atractylodis Macrocephalae Rhizoma with soil,46 components of Deep-fried Atractylodis Macrocephalae Rhizoma and 48 components of bleaching Atractylodis Macrocephalae Rhizoma.The results of PCA and PLS-DA showed that there were significant differences in the contents of the chemical components of Atractylodis Macrocephalae Rhizoma before and after processing,and 23 differential components such as atractylenolide I,atractylenolide II atrac-tylenolideⅢand biatractylolide were screened.Co

关 键 词：白术 炮制 化学成分 超高效液相色谱-四级杆-飞行时间串联质谱法(UPLC-Q-TOF-MS) 多元统计分析 

分 类 号：R283[医药卫生—中药学] R284.1[医药卫生—中医学]