液相色谱-四极杆/飞行时间质谱法快速筛查测定药物中芬太尼类物质

引用本文: 邓慧芬, 张建莹, 卞学海, 罗耀, 赵祥龙. 液相色谱-四极杆/飞行时间质谱法快速筛查测定药物中芬太尼类物质[J]. 色谱, 2020, 38(8): 906-913. doi: 10.3724/SP.J.1123.2019.11010 shu

Citation: DENG Huifen, ZHANG Jianying, BIAN Xuehai, LUO Yao, ZHAO Xianglong. Rapid screening and determination of fentanyl and its analogues in drugs by liquid chromatography- quadrupole time-of-flight mass spectrometry[J]. Chinese Journal of Chromatography, 2020, 38(8): 906-913. doi: 10.3724/SP.J.1123.2019.11010 shu

液相色谱-四极杆/飞行时间质谱法快速筛查测定药物中芬太尼类物质

邓慧芬 ^1, ,
张建莹 ^{1,
,} ,
卞学海 ^1, ,
罗耀 ^1, ,
赵祥龙 ^2,

1.
深圳海关食品检验检疫技术中心, 广东深圳 518045;
2.
AB SCIEX亚太应用中心, 上海 201206

通讯作者: 张建莹, E-mail:zhangjianying1001@163.com

基金项目:
海关总署项目（2019HK003）.

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5.00~100 μg/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10.0 μg/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。

关键词:

English

Rapid screening and determination of fentanyl and its analogues in drugs by liquid chromatography- quadrupole time-of-flight mass spectrometry

1.
Food Inspection & Quarantine Center, Shenzhen Customs, Shenzhen 518045, China;
2.
AB SCIEX Pacific Application Support Center, Shanghai 201206, China

Corresponding author: ZHANG Jianying, zhangjianying1001@163.com

Received Date: 04 December 2019
Fund Project:
China Customs Project (No. 2019HK003).

Abstract: 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 5.00-100 μg/L, with the correlation coefficients (r²)>0. 99. The limits of quantification for the 27 target compounds were 10.0 μg/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.

Key words:

liquid chromatography-quadrupole time-of-flight mass spectrometry (LC-QTOF-MS)
/ high resolution mass spectrometry (HRMS)
/ fentanyl and its analogues
/ drugs
/ screening

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1.
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液相色谱-四极杆/飞行时间质谱法快速筛查测定药物中芬太尼类物质

通讯作者: 张建莹, E-mail:zhangjianying1001@163.com

English

Rapid screening and determination of fentanyl and its analogues in drugs by liquid chromatography- quadrupole time-of-flight mass spectrometry

Corresponding author: ZHANG Jianying, zhangjianying1001@163.com

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

液相色谱-四极杆/飞行时间质谱法快速筛查测定药物中芬太尼类物质

通讯作者: 张建莹, E-mail:zhangjianying1001@163.com

English

Rapid screening and determination of fentanyl and its analogues in drugs by liquid chromatography- quadrupole time-of-flight mass spectrometry

Corresponding author: ZHANG Jianying, zhangjianying1001@163.com

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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