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。
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, 1.7 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.
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