基于化学计量学的川贝母药材及其混伪品平贝母的鉴别方法的建立
Establishment of identification method for Fritillariae Cirrhosae Bulbus and its adulterant Fritillariae Ussuriensis Bulbus based on chemometrics
石岩 1刘薇 1魏锋 1马双成1
作者信息
- 1. 中国食品药品检定研究院,北京 102629
- 折叠
摘要
目的:建立能够鉴别川贝母及其混伪品平贝母的方法.方法:使用化学计量学技术对样品四极杆串联飞行时间(Q TOF)质谱仪测定数据进行分析,并结合三重四极杆质谱筛选出特征离子对为m/z 578.3→164.14和m/z 578.3→398.31.采用 Waters Acquity UPLC CSH(75 mm ×2.1 mm,1.7 μm)色谱柱,以乙腈-0.1％甲酸溶液为流动相,流速0.4 mL·min-1.三重四极杆质谱仪MRM模式检测m/z 578.3→164.14和m/z 578.3→398.31 2个离子对.结果:108批样品的验证结果表明,m/z 578.3→164.14和m/z 578.3→398.31 2个特征离子对能够有效区分川贝母及其混伪品平贝母.结论:方法有较好的专属性和灵敏度,可用于平贝母掺伪川贝母的检测.
Abstract
Objective:To establish a method for identifying Fritillariae Cirrhosae Bulbus and its adulterant Fritillari-ae Ussuriensis Bulbus.Methods:Chemometrics techniques were used for the analysis of the sample data from deter-mination with Q TOF MS,and characteristic ion pairs were selected as m/z 578.3→164.14 and m/z 578.3→398.31 with triple quadrupole mass spectrometry applied,respectively.Then a specific approach was developed which used Waters Acquisition UPLC CSH(75 mm × 2.1 mm,1.7 μm)as column,and with acetonitrile and 0.1％formic acid solution as the mobile phase,and a flow rate of 0.4 mL·min-1.Two ion pairs:m/z 578.3→164.14 and m/z 578.3 →398.31 were detected by triple quadrupole mass spectrometer with MRM mode.Results:The validation results through 108 batches of samples indicated that the two characteristic ion pairs,m/z 578.3→164.14 and m/z 578.3→398.31,could effectively distinguish between Fritillariae Cirrhosae Bulbus and its adulterant Fritillariae Ussuriensis Bulbus.Conclusion:The method had good specificity and sensitivity,and could be used for the detection of adulterated Fritillariae Cirrhosae Bulbus with Fritillariae Ussuriensis Bulbus.
关键词
川贝母/平贝母/化学计量学/正交偏最小二乘判别分析/伪品鉴别/液质联用法/数据分析/特征筛选/特征离子Key words
Fritillariae Cirrhosae Bulbus/Fritillariae Ussuriensis Bulbus/chemometrics/OPLS-DA/counterfeit identification/LC-MS method/data analysis/feature screening/characteristic ion引用本文复制引用
出版年
2024
NETL
NSTL
万方数据