摘要
目的:采用超高效液相色谱-四极杆-飞行时间串联质谱法(UPLC-Q-TOF-MS)对茅苍术生品及米泔水制品的成分进行快速分析及鉴定,找出其炮制前后差异性成分。方法:运用TitanK C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(负离子模式:0~0.01 min,10%B;0.01~12 min,10%~25%B;12~18 min,25%~55%B;18~30 min,55%~70%B;30~35 min,70%~95%B;35~37 min,95%B;37~37.1 min,95%~10%B。正离子模式:0~0.01 min,10%B;0.01~10 min,10%~56%B;10~30 min,56%~75%B;30~35 min,75%~95%B;35~37 min,95%B;37~37.1 min,95%~10%B),正、负离子模式检测,电喷雾离子源(ESI),扫描范围m/z 100~1 250。结合对照品、数据库及相关文献信息,运用PeakView^(TM) 1.2软件对茅苍术及其米泔水制品进行化学成分鉴定。各样品数据经MarkerView1.2.1归一化处理后导入SIMCA 14.1中进行主成分分析(PCA)及正交偏最小二乘法-判别分析(OPLS-DA),通过变量重要性投影(VIP)值>1且t检验中P<0.01的原则,筛选得到茅苍术炮制前后差异性成分。结果:从茅苍术生品及米泔水制品中共鉴定得到56个成分,包括萜类17个、聚乙炔类8个、有机酸12个、糖苷类4个、黄酮类4个及其他类11个,两者共有成分43个,特有成分分别为7、6个。PCA及OPLS-DA结果表明,茅苍术炮制前后化学成分含量存在明显差异,共筛选得到苍术素、白术内酯Ⅰ、白术内酯Ⅱ及汉黄芩素等23个差异性成分。结论:茅苍术中主要含有倍半萜类、聚乙炔类及有机酸类成分,其炮制前后成分发生了水解等反应,且苍术素等有效成分含量增加,可为茅苍术炮制增效的物质基础研究提供参考。
Objective:To quickly analyze and identify the components in raw and rice-washed water products of Atractylodes lancea rhizoma(ALD)by ultra-high performance liquid chromatography quadrupoletime-of-flight mass spectrometry(UPLC-Q-TOF-MS),and then find out the differential components before and after processing.Method:TitanK Ccolumn(2.1 mm×100 mm,1.8 μm)was used with 0.1% formic acid aqueous solution(A)-acetonitrile(B)for gradient elution(0-0.01 min,10%B;0.01-12 min,10%-25%B;12-18 min,25%-55%B;18-30 min,55%-70%B;30-35 min,70%-95%B;35-37 min,95%B;37-37.1 min,95%-10%B under negative ion mode and 0-0.01 min,10%B;0.01-10 min,10%-56%B;10-30 min,56%-75%B;30-35 min,75%-95%B;35-37 min,95%B;37-37.1 min,95%-10%B under positive ion mode).Electrospray ionization was selected for collection and detection in positive and negative ion modes with the scanning range of m/z 100-1 250.Combining the reference substances,databases and related literature information,PeakView^(TM) 1.2software was used to identify the chemical components of ALD and its rice-washed water products.After normalized treatment by MarkerView1.2.1,the MS data of each sample were analyzed with principal component analysis(PCA)and orthogonal partial least squares-discriminant analysis(OPLS-DA)in SICMA14.1,and then the differential components before and after processing were screened according to the principle of variable importance in the projection(VIP)value>1 and P<0.01 in t-test.Result:A total of 56 components were identified from the raw and rice-washed water products of ALD,including 17 terpenoids,8polyacetylenes,12 organic acids,4 glycosides,4 flavonoids and 11 others.There were 43 components in both,and 7 and 6 specific components respectively.The results of PCA and OPLS-DA showed that there were significant differences in the contents of the chemical components of ALD before and after processing,and 23 differential components such as atractylodin,atractylenolide Ⅰ,atractylenolide Ⅱ and wogonin were screened.Conclusion:ALD mainly contains sesquiterpenoids,polyacetylenes and organic acids.The components of ALD are hydrolyzed before and after processing,and the content of active ingredients such as atractylodin increased.According to this,it can provide reference for the research on material basis of processing of ALD.
作者
王蝉
向茜
赵文燕
龚千锋
于欢
WANG Chan;XIANG Qian;ZHAO Wen-yan;GONG Qian-feng;YU Huan(School of Pharmacy,Jiangxi University of Chinese Medicine,Nanchang 330004,China)
出处
《中国实验方剂学杂志》
CAS
CSCD
北大核心
2022年第23期164-173,共10页
Chinese Journal of Experimental Traditional Medical Formulae
基金
国家自然科学基金项目(81960716)
国家中药标准化建设项目(ZYBZH-Y-JX-27)。
关键词
茅苍术
中药炮制
化学成分
米泔水
苍术素
白术内酯
超高效液相色谱-四极杆-飞行时间串联质谱法(UPLC-Q-TOF-MS)
Atractylodes lancea rhizoma
processing of traditional Chinese medicine
chemical compositions
rice-washed water
atractylodin
atractylenolide
ultra-high performance liquid chromatography quadrupole-time-of-flight mass spectrometry(UPLC-Q-TOF-MS)
