首页|喹啉羧酸共价有机框架微球在线固相萃取4种黄曲霉毒素

喹啉羧酸共价有机框架微球在线固相萃取4种黄曲霉毒素

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以1,3,5-三(4-氨基苯基)苯、联苯二甲醛、丙酮酸为合成反应单体,氨基磺酸为催化剂,利用Doebner串联反应成功制备了具有喹啉羧酸骨架的共价有机框架(QCA-COF)微球。通过优化反应条件发现,采用1,4-二氧六环-乙腈溶液(1∶4,体积比)作为反应溶剂时,可获得具有微米级粒径的微球。采用扫描电子显微镜、红外光谱、X射线粉末衍射、N2吸脱附实验对QCA-COF微球的结构进行表征。由于QCA-COF微球具有芳环、喹啉基团、羧基等官能团,可通过氢键、π-π等多重相互作用与黄曲霉毒素进行吸附,其吸附能力优于C18、PSA以及GCB等商用材料。将QCA-COF材料作为在线固相萃取柱的填料,详细优化了在线固相萃取条件。将在线固相萃取柱与高效液相色谱联用,建立了 4种黄曲霉毒素的检测方法,检出限为0。024~0。030 ng·g-1。经方法学验证,该方法具有较好的回收率(82。5%~105%)和精密度(4。3%~10%,n=6),适用于花生、小麦、陈皮、杏仁、决明子等食品与中药材中4种黄曲霉毒素的测定。
Quinolinecarboxylic Acid-linked Covalent Organic Framework Microsphere for On-line Solid Phase Extraction of Four Aflatoxins
In this study,on-line solid phase extraction(SPE)based on quinolinecarboxylic acid-linked covalent organic framework(QCA-COF)microsphere was developed.On-line SPE coupled with high performance liquid chromatography(HPLC)was used for the determination of four aflatoxins(AFs)in food samples and Chinese medicinal herbs,including AFB1,AFB2,AFG1 and AFG2.QCA-COF microsphere was successfully synthesized via the Doebner multicomponent reaction.For this process,1,3,5-tris(4-aminophenyl)benzene,4,4'-biphenyldicarboxaldehyde and pyruvic acid were used as the synthetic monomer under the catalysis of sulfamic acid.QCA-COF microsphere was characterized by scanning electron microscope,Fourier transform infrared spectroscopy,pow-der X-ray diffraction,and N2 adsorption-desorption isotherms.The results showed that micro-sized QCA-COF microsphere was obtained in a solution of 1,4-dioxane-acetonitrile(1∶4,volume ra-tio).The structure of QCA-COF has aromatic rings,pyridine groups and—COOH groups,which permits multiple binding interactions with aflatoxins.Based on their binding groups,QCA-COF ex-hibited excellent on-line SPE capability compared to the commercial materials,such as C18,PSA and GCB.The extraction parameters of the adsorption and elution processes were optimized in detail,including flow rates of loading,eluting solvent,volume of eluting solvent,and flow rates of elution.The optimal conditions were shown as follows:loading flow rate,0.4 mL·min-1;eluting solvent,300 μL of 0.1%acetic acid in methanol;elution flow rate,0.2 mL·min-1.Under the optimized conditions,the developed on-line SPE coupled with HPLC method provided good recovery(82.5%-105%),good precision(4.3%-10%,n=6),and low limit of detection(0.024-0.030 ng·g-1).The intro-duced method was successfully used to analyze four AFs in peanuts,wheat,orange peel,almonds and cassia seed.

aflatoxinson-line solid phase extractioncovalent organic frameworkhigh perfor-mance liquid chromatography

王荣雨、刘杰、周静、李涛、王晓、纪文华

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齐鲁工业大学(山东省科学院)山东省分析测试中心 天然产物分离提取共性技术创新与应用山东省工程研究中心,山东 济南 250014

山东明仁福瑞达制药股份有限公司,山东 济南 250014

山东蓝城分析测试有限公司,山东 济南 250100

黄曲霉毒素 在线固相萃取 共价有机框架 高效液相色谱

2025

分析测试学报
中国广州分析测试中心,中国分析测试协会

分析测试学报

北大核心
影响因子:1.498
ISSN:1004-4957
年,卷(期):2025.44(1)