Akter Mou Salma, Islam Rafiza, Shoeb Mohammad, Nahar Nilufar
Department of Chemistry University of Dhaka Dhaka Bangladesh.
Food Sci Nutr. 2021 Aug 16;9(10):5670-5675. doi: 10.1002/fsn3.2530. eCollection 2021 Oct.
Chloramphenicol (CAP), a bacteriostatic antibiotic, is used for the treatment of bacterial infections in human and animals. Continual exposure of CAP residues into animal tissues may lead to antibiotic resistance. For the protection of humans and animals from this problem, a fast and highly sensitive analytical method based on ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) was developed and validated in this study for the quantitative determination of CAP in poultry meat and beef samples. Quick, easy, cheap, effective, rugged, and safe (QuEChERS) method was used for the extraction of CAP residues. The developed method was validated in terms of linearity, accuracy, precision, and specificity. Poultry meat and beef samples were extracted with 20 ml water-acetonitrile (1:1, v/v) and cleaned up by MgSO, primary secondary amine, and C18 powder. The method was found to be linear in a wide concentration range, with correlation coefficient of higher than 0.999. The repeatability and reproducibility of this method were satisfactory. The achieved limit of detection and limit of quantification were 0.16 and 0.50 ng/g, respectively. Recoveries were estimated at 5 and 10 ng/g spiking levels in the range of 99%-111% with the coefficient of variation 0.48%-12.48% for spiked samples, and the matrix enhancement effects were mild in the range of 80%-85%. In this study, the levels of CAP residue in tested real samples were found below the detection limit. The method proved to be suitable for CAP determination in all kinds of samples tested and also efficient for the application of routine analysis.
氯霉素（CAP）是一种抑菌性抗生素，用于治疗人和动物的细菌感染。CAP残留持续进入动物组织可能导致抗生素耐药性。为保护人类和动物免受此问题影响，本研究开发并验证了一种基于超高效液相色谱 - 串联质谱法（UHPLC-MS/MS）的快速且高灵敏度分析方法，用于定量测定禽肉和牛肉样品中的CAP。采用快速、简便、廉价、有效、耐用且安全（QuEChERS）的方法提取CAP残留。所开发的方法在线性、准确度、精密度和特异性方面进行了验证。禽肉和牛肉样品用20毫升水 - 乙腈（1:1，v/v）提取，并用硫酸镁、伯仲胺和C18粉末净化。该方法在较宽浓度范围内呈线性，相关系数高于0.999。该方法的重复性和再现性令人满意。实现的检测限和定量限分别为0.16和0.50纳克/克。在5和10纳克/克的加标水平下，回收率估计在99% - 111%范围内，加标样品的变异系数为0.48% - 12.48%，基质增强效应在80% - 85%范围内较为温和。在本研究中，测试的实际样品中CAP残留水平低于检测限。该方法被证明适用于所测试的各类样品中CAP的测定，并且对于常规分析的应用也很有效。
