首页|基于UFLC-QTrap-MS/MS结合多元统计分析的不同产地、不同部位乌药中核苷和氨基酸类成分分析

基于UFLC-QTrap-MS/MS结合多元统计分析的不同产地、不同部位乌药中核苷和氨基酸类成分分析

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本研究建立了一种超快速液相色谱-三重四极杆/线性离子阱-串联质谱(UFLC-QTrap-MS/MS)同时测定乌药中11种核苷类和14种氨基酸类成分的分析方法,并结合多元统计分析比较不同产地、不同部位乌药的质量.采用Waters XBridge Amide色谱柱(2.1 mm× 100 mm×3.5 μm),以0.2％甲酸水溶液(A)-0.2％甲酸乙腈溶液(B)为流动相进行梯度洗脱;在电喷雾正离子模式下,以多反应监测(MRM)进行质谱检测;基于各成分的质量浓度,用方差分析(ANOVA)、主成分分析(PCA)、正交偏最小二乘法判别分析(OPLS-DA)、层次聚类分析(HCA)、逼近理想解排序法(TOPSIS)以及灰色关联度分析(GRA),对不同产地、不同部位乌药样品进行综合评价.结果表明,所测成分在一定浓度范围内具有良好的线性关系,相关系数均大于0.992 4;精密度、重复性、稳定性良好,平均加样回收率为94.86％～106.47％,相对标准偏差(RSD)均小于4.55％.不同产地、不同部位乌药样品间存在一定的差异,HCA和PCA 2种方法均将样品分为3类.OPLS-DA模型分析通过VIP值共筛选得到6个差异性化合物,分别为尿苷、丙氨酸、胞嘧啶、黄嘌呤、腺嘌呤、鸟嘌呤.该方法简便、灵敏度高、重现性好,可用于乌药中核苷和氨基酸类成分的同时测定,为药材质量评价和综合利用提供方法参考.
Analysis of Nucleosides and Amino Acids in Different Parts of Lindera aggregata(Sims)Kosterm.from Different Habitats by UFLC-QTrap-MS/MS Combined with Multivariate Statistical Analysis
A method of ultra-fast liquid chromatography-triple quadrupole/linear ion trap tandem mass spectrometry(UFLC-QTrap-MS/MS)was established for simultane-ous determination of 11 nucleosides and 14 amino acids in Lindera aggregata(Sims)Kosterm.,which combined with multivariate statistical analysis to evaluate the quality of different medication parts of Lindera aggregata(Sims)Kosterm.from different habitats.The gradient separation was performed on a Waters XBridge Amide column(2.1 mm× 100 mm × 3.5 μm)with 0.2％formic acid in water(A)and 0.2％formic acid in acetonitrile(B)as the mobile phase,and the mass spectrometric detection was carried out in electrospray positive ion mode under multiple reaction monitoring(MRM)mode.The samples of different habitats and medication parts were comprehensively evaluated by entropy weight ANOVA,PCA,OPLS-DA,HCA,TOPSIS and GRA according to the contents of 25 target constituents.All of the analytes had good linearity in the range of tested concentration with the correlation coefficient not less than 0.992 4.The average recoveries were between 94.86％and 106.47％,with the relative standard deviation(RSD)less than 4.55％.The analysis results showed that there were significant variations among the different medication parts of Lindera aggregata(Sims)Kosterm.samples.The contents of nucleosides and amino acids in tuber were signifi-cantly higher than those in taproot and leaf(p＜0.05).In terms of nucleoside,tuber had the highest content with an average content of 74.786 μg/g,followed by leaf of 55.401 μg/g and taproot of 36.290 μg/g.The highest content of amino acid was found in tuber with an average content of 50.850 μg/g,followed by the taproot and leaf with an average contents of 43.213 μg/g and 35.676 μg/g,respectively.The samples collect-ed from different parts of Lindera aggregata(Sims)Kosterm.in different regions were classified into three clusters by HCA and PCA according to the contents of nucleotides and amino acids detected.The classification results were satisfactory,indicating that there were obvious differences in the content of nucleosides and amino acids in different parts of the samples.Six different chemicals,namely uridine,alanine,cytosine,xanthine,adenine and guanine,were obtained by VIP co-screening in OPLS-DA model analysis.Comparing the maximum difference values of TOPSIS and GRA,it was found that the maximum difference value of ri in GRA was 12.08％,while Ci in TOPSIS was 53.23％.This method is simple,sensitive and accurate,which provides a reliable and effective technique for the quality control of Lindera aggregata(Sims)Kosterm..

ultra-fast liquid chromatography-triple quadrupole/linear ion trap mass spectrometry(UFLC-QTrap-MS/MS)Lindera aggregata(Sims)Kosterm.amino acidnucleosidedifferent habitatsdifferent parts

罗益远、顾海燕、谢叶菲、蒋新苗、王娟、蔡红蝶、马舒伟、陈宏降

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浙江药科职业大学中药学院,浙江宁波 315100

启东市人民医院药剂科,江苏南通 226299

超快速液相色谱-三重四极杆/线性离子阱-串联质谱(UFLC-QTrap-MS/MS) 乌药 氨基酸 核苷 不同产地 不同部位

浙江省公益基础研究项目浙江省药品监督管理局科技项目浙江省药品监督管理局科技项目浙江省医药卫生科技计划宁波市自然科学基金宁波市公益性科技计划浙江省教育厅一般项目浙江药科职业大学校级项目浙江药科职业大学校级项目

LTGN23H280002202200920230142023KY2982023J3062021S144Y20225021720221282022134

2024

10.7538/zpxb.2023.0049

质谱学报
北京中科科仪技术发展有限责任公司 中国物理学会质谱分会

质谱学报

CSTPCD北大核心EI
影响因子：1.046
ISSN：1004-2997
年,卷(期)：2024.45(2)
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