Chang Liming, Du Sishi, Wu Xiaojiao, Zhang Jian, Gan Zhiwei
Department of Pharmacy, West China Hospital, Sichuan University, Chengdu 610041, China.
College of Architecture and Environment, Sichuan University, Chengdu 610065, China.
Antibiotics (Basel). 2023 Jun 29;12(7):1125. doi: 10.3390/antibiotics12071125.
An optimized QuEChERS method for the simultaneous extraction of 26 antibiotics and 19 anthelmintics in whole cow milk was established, followed by UHPLC-MS/MS analysis. Briefly, 20 mL acetonitrile with 1 g disodium hydrogen citrate, 2 g sodium citrate, 4 g anhydrous MgSO, and 1 g sodium chloride were added to 10 g milk for target chemical extraction, followed by 50 mg anhydrous MgSO for purification. Satisfactory recoveries were obtained using the modified QuEChERS method, with recoveries of the antibiotics ranging from 79.7 to 117.2%, with the exception of norfloxacin, which was at 53.4%, while those for anthelmintics were in the range of 73.1-105.1%. The optimized QuEChERS method presented good precision, with relative standard deviations ranging from 7.2 to 18.6% for both antibiotics and anthelmintics. The method was successfully applied to analyze the antibiotics and anthelmintics in 56 whole cow milk samples from China. Briefly, the detection frequencies and concentrations of most of the antibiotics and anthelmintics were low in the whole cow milk samples, with concentrations ranging from below LOD to 4296.8 ng/kg. Fenbendazole, febantel, enrofloxacin, levofloxacin, sulfadiazine, and sulfamethoxazole were the predominant drug residues in the whole cow milk samples. Spatial distribution was found for those antibiotics and anthelmintics with detection frequency higher than 50%, especially for the antibiotics, indicating regional differences in drug application. Based on the current study, exposure to antibiotics and anthelmintics through whole cow milk consumption are lower than the acceptable daily intake values suggested by the China Institute of Veterinary Drug Control. However, long-term exposure to low doses of antibiotics and anthelmintics still needs attention and merits further study.
建立了一种优化的QuEChERS方法，用于同时提取全脂牛奶中的26种抗生素和19种驱虫药，随后进行超高效液相色谱-串联质谱（UHPLC-MS/MS）分析。简要地说，向10 g牛奶中加入20 mL乙腈以及1 g柠檬酸二钠、2 g柠檬酸钠、4 g无水硫酸镁和1 g氯化钠进行目标化学物提取，再加入50 mg无水硫酸镁进行净化。使用改进的QuEChERS方法获得了满意的回收率，抗生素的回收率在79.7%至117.2%之间，但诺氟沙星除外，其回收率为53.4%，驱虫药的回收率在73.1%至105.1%之间。优化的QuEChERS方法具有良好的精密度，抗生素和驱虫药的相对标准偏差均在7.2%至18.6%之间。该方法成功应用于分析来自中国的56份全脂牛奶样品中的抗生素和驱虫药。简要地说，全脂牛奶样品中大多数抗生素和驱虫药的检测频率和浓度较低，浓度范围从低于检测限到4296.8 ng/kg。芬苯达唑、非班太尔、恩诺沙星、左氧氟沙星、磺胺嘧啶和磺胺甲恶唑是全脂牛奶样品中的主要药物残留。发现检测频率高于50%的那些抗生素和驱虫药存在空间分布，尤其是抗生素，这表明药物使用存在区域差异。基于当前研究，通过食用全脂牛奶接触抗生素和驱虫药的情况低于中国兽医药品监察所建议的每日可接受摄入量值。然而，长期接触低剂量的抗生素和驱虫药仍需关注且值得进一步研究。
