Guangdong Provincial Key Laboratory of Nutraceuticals and Functional Foods, College of Food Science, South China Agricultural University, Guangzhou, Guangdong, 510642, China; Guangdong Engineering and Technology Research Center for Ambient Mass Spectrometry, Guangdong Provincial Key Laboratory of Emergency Test for Dangerous Chemicals, Guangdong Institute of Analysis (China National Analytical Center Guangzhou), Guangzhou, 510070, China.
Guangdong Engineering and Technology Research Center for Ambient Mass Spectrometry, Guangdong Provincial Key Laboratory of Emergency Test for Dangerous Chemicals, Guangdong Institute of Analysis (China National Analytical Center Guangzhou), Guangzhou, 510070, China.
Talanta. 2019 Nov 1;204:238-247. doi: 10.1016/j.talanta.2019.05.102. Epub 2019 May 28.
In this article, an ambient mass spectrometric method with molecularly imprinted polymer (MIP)-coated wooden tips was developed for sensitive analysis of trace macrolide antibiotics in complex food samples. A novel solid-phase microextraction (SPME) probe was prepared, via the modification of a layer MIP coating (with roxithromycin as template molecule) on the surface of wooden tips. The obtained MIP-coated wooden-tip SPME probe can be applied directly to enrich trace macrolide antibiotics from complex food samples, with enrichment factors of 244-1604, 72-370, and 12-82 folds for analysis of five investigated macrolide antibiotics in drinking water, honey, and milk samples, respectively. After extraction, a high voltage and some spray solvent were applied on the loaded SPME probe to desorb and ionize analytes enriched on the probe surface for electrospray ionization mass spectrometric (ESI-MS) analysis under ambient and open-air conditions. The method showed good linearity, with correlation coefficient values (r) no less than 0.9904, and the calibration function was verified via Mandel's fitting test (p > 0.063). The limits of detection were in the range of 0.003-0.05, 1.1-5.1, and 1.9-15.8 ng/g for analysis of drinking water, honey, and milk samples, respectively. Recoveries of the five targeted macrolide antibiotics in honey and milk samples ranged from 73.4% to 98.1%, with the standard deviations no higher than 8.6%. As a result, MIP-coated wooden-tip ESI-MS method could be feasibly used as a sensitive method for determination of trace macrolide antibiotics in complex food samples.
本文开发了一种基于分子印迹聚合物（MIP）涂层木尖的环境质谱分析方法，用于灵敏分析复杂食品样品中的痕量大环内酯类抗生素。通过在木尖表面修饰一层 MIP 涂层（以罗红霉素为模板分子），制备了新型固相微萃取（SPME）探针。所得 MIP 涂层木尖 SPME 探针可直接用于从复杂食品样品中富集痕量大环内酯类抗生素，对饮用水、蜂蜜和牛奶样品中五种被研究的大环内酯类抗生素的分析，其富集因子分别为 244-1604、72-370 和 12-82 倍。萃取后，在加载的 SPME 探头上施加高电压和一些喷雾溶剂，以在环境和开放空气中对探针表面上富集的分析物进行解吸和离子化，用于电喷雾电离质谱（ESI-MS）分析。该方法表现出良好的线性，相关系数（r）值不低于 0.9904，通过曼德尔拟合检验（p>0.063）验证了校准函数。对于饮用水、蜂蜜和牛奶样品的分析，检测限分别在 0.003-0.05、1.1-5.1 和 1.9-15.8 ng/g 范围内。在蜂蜜和牛奶样品中，五种目标大环内酯类抗生素的回收率在 73.4%-98.1%之间，标准偏差不高于 8.6%。因此，MIP 涂层木尖 ESI-MS 方法可作为一种灵敏的方法，用于复杂食品样品中痕量大环内酯类抗生素的测定。
