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

作　　者：石岩[1] 刘薇[1] 魏锋[1] 马双成[1] SHI Yan;LIU Wei;WEI Feng;MA Shuang-cheng(National Institutes for Food and Drug Control,Beijing 102629,China)

机构地区：[1]中国食品药品检定研究院,北京102629

出　　处：《药物分析杂志》2024年第7期1222-1232,共11页Chinese Journal of Pharmaceutical Analysis

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,1.7μm)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.

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 

分 类 号：R917[医药卫生—药物分析学]