摘要
基于液相色谱-四极杆/飞行时间质谱(LC-QTOF-MS)建立了药物中27种新型毒品芬太尼类物质(芬太尼及其类似物)的同时快速筛查、确证和定量分析方法。样品经5 mL 75%(v/v)乙腈水溶液和5 mL乙腈提取,HLB固相萃取柱净化,电喷雾电离,正离子扫描,TOF-MS和信息依赖性采集(IDA)-MS/MS采集模式检测,外标法定量;建立一级精确质量数据库、保留时间和二级质谱库,实现了固体压片、粉末、液体药物及透皮贴剂中27种芬太尼类物质的快速筛查和确证。在5.00~100μg/L范围内,27种目标化合物的线性关系良好(r2>0.99)。27种化合物的定量限均为10.0μg/kg。在维生素C压片、头痛粉、止咳水、透皮贴剂样品中3个添加水平的平均回收率范围分别82.9%~106%、84.8%~106%、86.9%~109%和83.1%~106%,相对标准偏差(RSD)为0.38%~8.71%(n=6)。本方法操作简便,耗时短,灵敏度高,稳定性好,适用于液体和固体药物中芬太尼类物质的筛查检测及定量分析,可显著降低检测成本,具有实际应用价值。
A method based on liquid chromatography coupled with high-resolution quadrupole time-of-flight mass spectrometry(LC-QTOF-MS)was developed for the simultaneous screening and determination of fentanyl and its 26 analogs in liquid and solid powder drugs.The established method involves successive extraction by 5 mL 75%(v/v)acetonitrile aqueous solution and 5 mL acetonitrile,followed by clean-up using the hydrophilic lipophilic balance(HLB)solid-phase extraction method.Detection was achieved by electrospray ionization(ESI)in the positive mode,TOF-MS,and information-dependent acquisition(IDA)-MS/MS acquisition;the external standard method was adopted for quantification.Two databases of accurate mass and fragment ions were created.The standard matrix-matched calibration curves of the 27 target compounds were linear in the range of 5.00-100μg/L,with the correlation coefficients(r2)>0.99.The limits of quantification for the 27 target compounds were 10.0μg/kg.The recoveries for all the target compounds in vitamin C tablet,headache powder,cough syrup,and transdermal patch samples were in the ranges of 82.9%-106%,84.8%-106%,86.9%-109%,and 83.1%-106%,respectively,with relative standard deviations ranging from 0.38%to 8.71%(n=6).The results demonstrated that the developed method is rapid and sensitive for the simultaneous monitoring and determination of fentanyl and 26 its analogs in liquid and solid powder drugs.
作者
邓慧芬
张建莹
卞学海
罗耀
赵祥龙
DENG Huifen;ZHANG Jianying;BIAN Xuehai;LUO Yao;ZHAO Xianglong(Food Inspection & Quarantine Center, Shenzhen Customs, Shenzhen 518045, China;AB SCIEX Pacific Application Support Center, Shanghai 201206, China)
出处
《色谱》
CAS
CSCD
北大核心
2020年第8期906-913,共8页
Chinese Journal of Chromatography
基金
海关总署项目(2019HK003)。
关键词
液相色谱-四极杆/飞行时间质谱
高分辨质谱
芬太尼类物质
药物
筛查
liquid chromatography-quadrupole time-of-flight mass spectrometry(LC-QTOF-MS)
high resolution mass spectrometry(HRMS)
fentanyl and its analogues
drugs
screening
