State Key Laboratory of Analytical Chemistry for Life Science, School of Chemistry and Chemical Engineering , Nanjing University , Nanjing 210023 , China.
Zhejiang Engineering Institute of Food Quality and Safety, School of Management and E-Business , Zhejiang Gongshang University , Hangzhou 310018 , China.
Anal Chem. 2019 Nov 5;91(21):13418-13426. doi: 10.1021/acs.analchem.9b01844. Epub 2019 Oct 15.
In this work, a highly integrated microfluidic chip with multifunction coupled to mass spectrometry (MS) was developed for online analysis of seven different regulated quinolones (QNs) in milk samples. Procedures of sample extraction, immunoaffinity enrichment, magnetic separation, and online elution were performed simultaneously on the specifically designed device. Based on the specificity of antibodies, direct (electrospray ionization) ESI-MS at full scan mode without liquid chromatography (LC) separation and further tandem mass spectrometry (MS/MS) analysis was developed for the identification of target QNs. One single isotope internal standard (IS) method was presented for quantitative analysis of seven QNs. Upon targeted online extraction and enrichment by antibody conjugated magnetic beads, seven QNs were quantitatively determined by the IS method with the linear range of 0.2/0.5-10 ng/mL ( > 0.991). The limits of detection (LODs) for the seven QNs were in the range of 0.047-0.490 ng/mL. This system permits automated on-chip immunoaffinity enrichment and accurate MS detection without additional off-line cleanup procedures.
本工作开发了一种高度集成的微流控芯片,与质谱(MS)联用,可在线分析牛奶样品中的七种不同的管制喹诺酮类药物(QNs)。在专门设计的装置上,同时进行样品提取、免疫亲和富集、磁分离和在线洗脱等操作。基于抗体的特异性,无需液相色谱(LC)分离,采用全扫描模式的直接(电喷雾电离)ESI-MS 以及进一步的串联质谱(MS/MS)分析,对目标 QNs 进行了鉴定。建立了一种单一同位素内标(IS)方法,用于七种 QNs 的定量分析。通过抗体偶联的磁性珠进行靶向在线提取和富集,七种 QNs 采用 IS 法进行定量分析,线性范围为 0.2/0.5-10 ng/mL(>0.991)。七种 QNs 的检出限(LODs)在 0.047-0.490 ng/mL 范围内。该系统允许在芯片上自动进行免疫亲和富集和准确的 MS 检测,无需额外的离线净化程序。