National Reference Laboratory of Veterinary Drug Residues (SCAU), College of Veterinary Medicine, South China Agricultural University, Guangzhou, China.
Guangdong Provincial Key Laboratory of Veterinary Pharmaceutics, Development and Safety Evaluation, South China Agricultural University, Guangzhou, China.
Anal Sci. 2021 Dec 10;37(12):1687-1693. doi: 10.2116/analsci.21P037. Epub 2021 May 21.
It is significant to develop a method for the simultaneous determination of multiple polypeptide antibiotics residues in lake water because of the emergence of multidrug-resistant microorganisms in water. A sensitive, eco-friendly and simple method was developed for the determination of multiple polypeptide antibiotics, including vancomycin, teicoplanin, polymyxin B, colistin and bacitracin A in lake water using liquid chromatography-tandem mass spectrometry (LC-MS/MS). Water samples were lyophilized to enrich them after adjusting the pH to 3. Then, 80% methanol in water containing 0.1% formic acid was used to reconstitute the residues for LC-MS/MS analysis. The results showed that target compounds were well separated and detected under the optimum instrumental conditions. The limits of detection and the limits of quantification of polypeptide antibiotics were in the range of 0.01 - 0.1 and 0.02 - 0.2 ng mL, respectively. The matrix-matched calibration curves of all compounds were linear in the calibration range of 1 - 200 ng mL. At three spiked levels of 0.2 (0.04), 0.4 (0.1) and 1.0 (0.2) ng mL in lake water, the average recoveries of analytes were higher than 70%, except for teicoplanin, with relative standard deviations of less than 20%. Compared with other common sample pretreatment methods, the lyophilization process is simpler and more eco-friendly, achieving the simultaneous detection of multiple polypeptide antibiotics in lake water. The developed method is successfully applied to the routine monitoring of polypeptide antibiotics residues in lake water.
由于水中多药耐药微生物的出现，开发一种同时测定多种多肽抗生素残留的方法具有重要意义。本研究建立了一种灵敏、环保、简单的同时测定水中万古霉素、替考拉宁、多黏菌素 B、黏菌素和杆菌肽 A 等多种多肽抗生素残留的方法，采用液相色谱-串联质谱法（LC-MS/MS）。水样 pH 调至 3 后冻干浓缩，然后用含 0.1%甲酸的 80%甲醇复溶，用于 LC-MS/MS 分析。结果表明，在最佳仪器条件下，目标化合物分离检测效果良好。多肽抗生素的检测限和定量限分别在 0.01-0.1 和 0.02-0.2ng/mL 范围内。所有化合物的基质匹配校准曲线在 1-200ng/mL 的校准范围内均呈线性。在湖水 0.2（0.04）、0.4（0.1）和 1.0（0.2）ng/mL 三个加标水平下，除替考拉宁外，各分析物的平均回收率均高于 70%，相对标准偏差均小于 20%。与其他常见的样品预处理方法相比，冻干过程更简单、更环保，实现了湖水中多种多肽抗生素的同时检测。该方法成功应用于湖水中多肽抗生素残留的常规监测。
