摘要
建立了液相色谱-四极杆/静电场轨道阱高分辨质谱法监测口服液中33种芬太尼类精神药物的定向自动筛查方法。样品在盐析的作用下,乙腈超声提取,固相基质分散净化,在电喷雾正离子模式下,一级四极杆质谱在m/z 2.0隔离窗口下过滤带电分子离子,高分辨静电场轨道阱质谱自动触发子离子全扫描分析,根据芬太尼的精确质量数、同位素丰度比、二级碎片离子建立标准物质数据库,采用Trace Finder 5.1软件自动检索匹配完成目标物的筛查。口服液中33种芬太尼类方法定量限为(LOQ)10μg/kg,分析物在5~200μg/kg浓度范围内线性关系良好,相关系数R^(2)≥0.9993;方法回收率在72.6%~102.4%之间,相对标准偏差为3.8%~10.5%。结果表明,所建立的筛查方法可用于口服液中33种芬太尼类精神药物的自动筛查与测定,具有准确、快速、实用的特点。
An analytical method has been developed for screening 33 fentanyl psychoactive substances in oral liquid by high performance liquid chromatography combined quadrupole-orbitrap high resolution mass spectrometry(Q/Exactive).With salting out,the samples were extracted by acetonitrile under the ultrasonic conditions and the purification were carried out with solid matrix dispersion.The positive ions were entered quadrupole mass limited to isolation window m/z 2.0 and the product ion scan was automatically performed on the full MS scan/data triggered mode.According to parameters of molecular ion,isotopic ion ratios,characteristic product ion,the searched database were built.Automatic screening was performed with the Trace Finder 5.1 software.Under the experimental conditions,the limits of quantification(LOQ)were 10μg/kg for 33 analysts.The good linear relationship was obtained at 5-200μg/kg(correlation coefficient R^(2)≥0.9993).The method recoveries were 72.6%-102.4%and the relative standard deviations(RSDs)were 3.8%-10.5%.The automatic screening method is fast,accurate,and practical,which can be used to screen and determine 33 fentanyl psychotropic drugs in oral liquid.
作者
祝伟霞
魏蔚
郁露
张淑霞
邢荣花
张卫理
ZHU Weixia;WEI Wei;YU Lu;ZHANG Shuxia;XING Ronghua;ZHANG Weili(Zhengzhou Customs Technology Centre,Zhengzhou 450009,Henan,China)
出处
《化学研究》
CAS
2023年第4期328-332,共5页
Chemical Research
基金
海关总署科研项目(2020HK227)。
关键词
液相色谱-高分辨质谱
保健品口服液
芬太尼类精神活性药物
自动筛查
high performance liquid chromatography-quadrupole/orbitrap high resolution mass spectrometry
oral liquid
fentanyl psychoactive substances
automatic screening
