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

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,1.7μm)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→398.312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→398.312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。

Objective:To establish a method for identifying Fritillariae Cirrhosae Bulbus and its adulterant Fritillariae Ussuriensis Bulbus.Methods:Chemometrics techniques were used for the analysis of the sample data from determination 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,1.7μm)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.