QuEChERS结合UPLC-Q-Orbitrap HRMS快速靶向筛查凉茶中非法添加140种药物  

QuEChERS combined with UPLC-Q-Orbitrap targeted rapid screening of illegally added 140 drugs in herbal tea

作　　者：杨乐[1] 易华娟 林秋凤[1] 刘丹丹[1] 郑耀林 张树权 魏志雄[1] YANG Le;YI Hua-Juan;LIN Qiu-Feng;LIU Dan-Dan;ZHENG Yao-Lin;ZHANG Shu-Quan;WEI Zhi-Xiong(Dongguan Institute for Food and Drug Control,Dongguan 523000,China)

机构地区：[1]东莞市食品药品检验所,东莞523808

出　　处：《实验室检测》2024年第9期1-8,共8页Laboratory Testing

基　　金：广东省市场监督管理局科研攻关项目(2023SC11);东莞市社会发展科技项目(20211800901872)

摘　　要：目的采用QuECHERS前处理技术,基于超高效液相色谱–四级杆–静电场轨道离子肼高分辨质谱法(Ultra performance liquid chromatography-quadrupole-electrostatic field orbitrap high resolution mass spectrometry,UPLC-QOrbitrap HRMS)建立快速靶向筛查凉茶中非法添加14类140种药物的分析检测方法。方法样品加甲醇提取,用无水硫酸镁–醋酸钠、十八烷基键合硅胶–中性氧化铝粉末进行分散固相萃取净化,用色谱柱Waters BEH C_(18)(2.1 mm×50 mm,1.7μm)分离,通过0.2%甲酸水(V/V)溶液–0.2%甲酸乙腈(V/V)溶液和水–乙腈两个独立的流动相体系梯度洗脱,数据采集模式Full MS/dd–MS^(2),配置阴性基质标准曲线并采用外标法定量。结果有代表性的20种质控化合物在5.0~200 ng/mL质量浓度范围内线性关系良好(r^(2)>0.995),低中高三水平加标量下的平均回收率为83.1%~107.3%,相对标准偏差RSD<15.6%,检出限0.2~1.0 mg/kg。对市场上165批凉茶进行测定,其中12批阳性被检出,阳性成分为氯苯那敏、对乙酰氨基酚、双氯芬酸纳、布洛芬、地塞米松醋酸酯、红霉素和氟甲砜霉素。结论该方法操作简单、灵敏度高、筛查通量高,适用于凉茶等保健食品中非法添加药物的检测。Objective Based on UHPLC-Orbitrap HRMS,combined with QuECHERS pretreatment technology,a rapid screening detection method was established to simultaneously screen and confirm 14 categories of 140 illegally added drugs in herbal tea.Methods The sample was extracted with methanol,and purified by dispersed solid phase extraction with sodium acetate and anhydrous magnesium sulfate,neutral alumina and octadecyl bonded silica gel,separated by a chromatographic column Waters BEH C_(18)(2.1 mm×50 mm,1.7μm),and gradient eluted by two independent mobile phase systems:0.2%formic acid water(V/V)solution~0.2%formic acid acetonitrile(V/V)solution and water-acetonitrile,Full MS/dd-MS^(2) mode was used to collect data,the standard curve was prepared by extracting solution from blank sample and the external standard method was used for quantification.Results The linear relationship of 20 representative quality control compounds was good(r^(2)>0.995)from 5.0 to 200 ng/mL mass concentration,the average recovery rateat the three levels of low,medium and high is between 83.1%and 107.3%,the relative standard deviation is less than 15.6%and detection low limit is between 0.2 mg/kg and 1.0 mg/kg.165 herbal tea samples on the market were determined and results showed that twelve samples were positive,the positive components were chlorpheniramine,acetaminophen,diclofenac sodium,ibuprofen,dexamethasone acetate,erythromycin and florfenicol.Conclusion The method has the advantages of simple operation,high sensitivity and highthroughput screening.Is suitable for the detection of illegally added drugs in herbal tea and other health foods.

关 键 词：非法添加 凉茶 靶向筛查 QUECHERS 超高效液相色谱–四级杆–静电场轨道肼高分辨质谱法 

分 类 号：O657.63[理学—分析化学] TS275.2[理学—化学]