基于UPLC-Q-TOF-MS、DESI-MSI法实时监测附子生长过程中不同部位多效唑变化  

Real-time monitoring of the paclobutrazol variations in different parts of Aconitum carmichaeli during its growth based on UPLC-Q-TOF-MS and DESI-MSI methods

作　　者：侯寓森 裴照卿 徐彬杰 唐策[3] HOU Yu-sen;PEI Zhao-qing;XU Bin-jie;TANG Ce(School of Pharmacy,Chengdu University of Traditional Chinese Medicine,Chengdu 611137,China;Innovative Institute of Chinese Medicine and Pharmacy,Chengdu University of Traditional Chinese Medicine,Chengdu 611137,China;School of Ethnic Medicine,Chengdu University of Traditional Chinese Medicine,Chengdu 611137,China)

机构地区：[1]成都中医药大学药学院,四川成都611137 [2]成都中医药大学中医药创新研究院,四川成都611137 [3]成都中医药大学民族医药学院,四川成都611137

出　　处：《中成药》2023年第8期2603-2608,共6页Chinese Traditional Patent Medicine

基　　金：国家自然科学基金(81903922);“杏林学者”青基人才专项项目(QJRC2022044)。

摘　　要：目的建立UPLC-Q-TOF-MS、DESI-MSI法实时监测附子生长过程中不同部位多效唑的变化,考察DESI-MSI法在分析多效唑过程中的优势。方法不同生长期、不同部位48批附子经QuEChERS提取后,采用UPLC-Q-TOF-MS和DESI-MSI法进行多效唑检测。DESI-MSI法技术参数为以90%甲醇-甲酸(1000∶0.5)为喷雾溶剂,体积流量2μL/min;扫描范围100~600 Da;空间分辨率120μm;锥孔电压80 V;喷雾器(N_(2))压力0.45 MPa;毛细管电压4.5 kV;离子源温度150℃;正离子扫描样本。结果种植附子的土壤中均含有多效唑,地上、地下部分分别发现有6、9批附子含有多效唑,DESI-MSI和UPLC-Q-TOF-MS法均能对其进行半定量分析,分析结果基本一致。同时,DESI-MSI法所用流动相体积和测试时间要明显少于UPLC-Q-TOF-MS法,并能对相对含量进行直观呈现。结论附子在种植过程中存在喷施多效唑的可能。本研究开发了一种结合DESI-MSI和UPLC-Q-TOF-MS技术快速检测附子不同部位多效唑的方法,为附子生长过程中多效唑的快速检测提供了参考。AIM To establish UPLC-Q-TOF-MS and DESI-MSI method to make the realtime monitoring of the paclobutrazol variations in different parts of Aconitum carmichaeli Debx.during its growth,and to investigate the advantage of DESI-MSI method in the qualitative and quantitative analyses of paclobutrazol.METHODS Forty-eight batches of A.carmichaeli of different growth stages and different parts extracted by QuEChERS had their content of paclobutrazol detected using UPLC-Q-TOF-MS and DESI-MSI method.The technical parameters of DESI-MSI method were 90%methanol formic acid(1000∶0.5)as the spray solvent,with the volume flowing at rate of 2μL/min;scanning range of 100-600 Da;spatial resolution of 120μm;cone hole voltage of 80 V;spray pressure(N_(2))of 0.45 MPa;capillary voltage of 4.5 kV;ion source temperature of 150℃;and positive ion scanning upon the samples.RESULTS A.carmichaeli found all of its growing soil,and six batches of its aboveground parts,nine batches of underground parts containing paclobutrazol.Although both DESI-MSI and UPLC-Q-TOF-MS method successfully performed semi quantitative analysis showing basically consistent result,DESI-MSI method required significantly less mobile phase volume and testing time,and displayed more apparent relative content.CONCLUSION The rapid detection of paclobutrazol,a misused substance during the growing period of A.carmichaeli,may be achieved through our developed method with the combination use of DESI-MSI and UPLC-Q-TOF-MS techniques.

关 键 词：附子 多效唑 实时监测 DESI-MSI UPLC-Q-TOF-MS 

分 类 号：R282[医药卫生—中药学]