摘要
建立了一种基于超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法(UPLC-Q/OrbitrapHRMS)快速筛查及定量分析清咽类保健食品中12种非法添加药物的方法。样品经乙腈超声提取,高速离心,以ZORBAXXDB-C_(18)(50mm×2.1mm,1.8μm)为色谱柱,甲醇与0.1%甲酸水溶液(含5mmol/L乙酸铵)为流动相,梯度洗脱,质谱采集用Q Extractive高分辨质谱中正离子扫描,一级全扫描和数据依赖的二级子离子扫描(Full MS/dd-MS^(2))监测模式,以Full MS提取高分辨母离子色谱峰的面积定量,以保留时间、一级母离子以及dd-MS^(2)扫描所得的二级碎片离子信息建立数据库定性筛查。12种药物在7.63min内的得到有效分离,精确质量数偏差不大于1.48×10^(-6),在1.00~200.00μg/L范围内线性关系良好(相关系数≥0.999),测定下限为50.00~150.00μg/kg,加标回收率在75.15%~117.65%之间,相对标准偏差(RSD)为0.89%~4.84%。该方法前处理简单、快速,分析检测准确,灵敏度高,选择性强,可用于清咽类保健食品中12种非法添加药物快速定性筛查和定量分析。
A method for rapid screening and quantitative analysis of 12 kinds of illegally added drugs in throat-cleaning healthcare food products based on ultra high performance liquid chromatography-quadrupole/elecrostatic orbitrap high resolution mass spectrometry(UPLC-Q/Orbitrap HRMS)was developed.The sample was extracted with acetonitrile and centrifuged at a high speed.The separation of the 12 target compounds was performed on a ZOBAX XDB-C_(18) column(50 mm×2.1 mm,1.8μm)through a gradient elution with 0.1%formic acid(containing 5 mmol/L ammonium acetate)and methanol as the mobile phase.Mass spectrometry analysis was performed via the full MS/dd-MS2 acquisition with positive ionization mode,and the chromatographic peak areas obtained through extracting the accurate mass number of parent ions by full MS first-order mass spectrometry were quantified.A database was established for qualitative screening based on the retention time,primary precursor mass and secondary fragment ions information from DD-MS2 scans.The 12 kinds of drugs were effectively separated within 7.63 min with the mass accuracy deviation lower than 1.48×10^(-6).A good linearity was obtained in the range from 1.00μg/L to 200.00μg/L,with a correlation coefficients higher than 0.999.The lower limits of detection ranged from 50.00μg/kg to 150.00μg/kg.The average spiked recoveries for 12 target compounds were between 75.15%and 117.65%,with relative standard derivations(RSDs)ranged from 0.89%to 4.84%.The method was simple,fast,accurate,sensitive and selective,thus can be used for rapid qualitative screening and quantitative analysis of illegally added chemical drugs in throat-cleaning healthcare food products.
作者
郭立净
袁利杰
袁阳蕾
GUO Lijing;YUAN Lijie;YUAN Yangei(Henan Institute of Food Inspection,Key Laboratory of Food Safety Quick Testing and Smart Supervision Technology for State Market Regulation,Special Food Engineering Technology Center,Zhengzhou 450003,China)
出处
《现代食品科技》
CAS
北大核心
2022年第12期375-382,共8页
Modern Food Science and Technology
基金
国家自然科学基金资助项目(21577042)
河南省市场监督管理局应用技术研究项目(2020sj36)。
关键词
保健食品
非法添加
高效液相色谱-四极杆/静电场轨道阱高分辨质谱
health food with effect of clearing the throat
illegally adulteration
ultra high performance liquid chromatography-quadrupole/elecrostatic orbitrap high resolution mass spectrometry(UPLC-Q/Orbitrap HRMS)
