Zhejiang Provincial Key Laboratory of Advanced Mass Spectrometry and Molecular Analysis, Institute of Mass Spectrometry, School of Material Science and Chemical Engineering, Ningbo University, Ningbo, Zhejiang, 315211, China.
Zhejiang Provincial Key Laboratory of Advanced Mass Spectrometry and Molecular Analysis, Institute of Mass Spectrometry, School of Material Science and Chemical Engineering, Ningbo University, Ningbo, Zhejiang, 315211, China.
Talanta. 2021 Mar 1;224:121402. doi: 10.1016/j.talanta.2020.121402. Epub 2020 Jul 18.
In this work, a sensitive, rapid, and matrix effect-free method for online simultaneous detection of benzimidazoles in animal products by in-tube solid-phase microextraction coupled with mass spectrometry (in-tube SPME-MS) was investigated. Herein, according to the chemical structures properites of the analyte benzimidazoles, poly (3-Acrylamidophenylboronic acid-co-divinylbenzene-co-N,N'-Methylenebisacryladmide) [poly (AAPBA-co-DVB-co-MBAA)] microextraction column was prepared, and severs as the extraction and enrichment medium (in-tube SPME) via hydrophobic, B-N coordination, π-π, and hydrogen bonding interactions with the benzimidazoles. The monolithic column was optimized and characterized, showing satisfactory permeability and extraction capacity in range of 514-1000 μg mL for the benzimidazoles. The important parameters of the in-tube SPME-MS system experimental condition were systematically optimized to achieve the maximal extraction efficiency. Under the optimized condition, the MS intensity of benzimidazoles measured by in-tube SPME-MS is more significant, cleaner, and has a better signal-to-noise ratio than the mass intensity measured by direct MS method. Good linearity was obtained with correlation coefficients between 0.9915 and 0.9990, and the detection limits (S/N = 3) of the benzimidazoles were between 0.55 and 0.91 ng g. Recoveries in the range of 72.5%-92.4% were obtained for the benzimidazoles in pork and chicken in three spiked concentration levels, with satisfactory relative standard deviations (n = 4) that lower than 7.5%. The developed in-tube SPME-MS method based on the poly (AAPBA-co-DVB-co-MBAA) column was successfully used to sensitively determine trace benzimidazoles in animal products without interference peaks, indicating that it is promising for the analysis of benzimidazoles in practical samples that requiring minimal sample pre-treatment and no chromatographic separation.
本文研究了一种在管固相微萃取-质谱联用（in-tube SPME-MS）在线同时检测动物产品中苯并咪唑类药物的灵敏、快速、无基质效应的方法。在此，根据分析物苯并咪唑类药物的化学结构特性，制备了聚（3-丙烯酰胺基苯硼酸-co-二乙烯基苯-co-N,N'-亚甲基双丙烯酰胺）[聚（AAPBA-co-DVB-co-MBAA）]微萃取柱，并通过疏水、B-N 配位、π-π 和氢键相互作用作为萃取和富集介质（in-tube SPME）与苯并咪唑类药物结合。对整体柱进行了优化和表征，在 514-1000μg/mL 范围内对苯并咪唑类药物具有良好的渗透性和萃取能力。系统优化了 in-tube SPME-MS 系统实验条件的重要参数，以达到最大的萃取效率。在优化条件下，通过 in-tube SPME-MS 测量的苯并咪唑类药物的 MS 强度比直接 MS 法测量的质量强度更显著、更干净、信噪比更好。苯并咪唑类药物的线性良好，相关系数在 0.9915 到 0.9990 之间，检测限（S/N=3）在 0.55 到 0.91ng/g 之间。在三个加标浓度水平下，猪肉和鸡肉中苯并咪唑类药物的回收率在 72.5%-92.4%之间，相对标准偏差（n=4）均低于 7.5%，结果令人满意。该方法基于聚（AAPBA-co-DVB-co-MBAA）柱的 in-tube SPME-MS 方法成功用于灵敏检测动物产品中的痕量苯并咪唑类药物，无干扰峰，表明该方法有望用于实际样品中苯并咪唑类药物的分析，无需样品预处理和色谱分离。
