Sun Feifei, Qiu Jicheng, Kong Jingyuan, Cao Yuying, Li Lin, Cao Xingyuan
Animal-Derived Food Safety Innovation Team, College of Animal Science and Technology, Anhui Agricultural University, Hefei, China.
Department of Veterinary Pharmacology and Toxicology, China Agricultural University, Beijing, China.
Front Vet Sci. 2024 Sep 3;11:1462743. doi: 10.3389/fvets.2024.1462743. eCollection 2024.
Enramycin, a common growth promoter utilized in chickens and pigs, is sensitive against Gram-positive bacteria, and the maximum residue limit (MRL) of enramycin set up by is 30 μg/kg. However, the methods have been reported for detecting enramycin have failed to meet the accuracy requirements, with the required limit of quantification being higher than the MRL. To address this issue, we developed a high-sensitive and robust analytical method based on ultrahigh-performance liquid chromatography coupled with mass spectrometry (UHPLC-MS/MS), to determine enramycin residues in swine tissues, including liver, kidney, pork, and fat. The ENV cartridge was selected to cleanup and enrich analytes after being extracted using a mixture of 55% methanol containing 0.2 M hydrochloric acid. With comprehensively validation, this established method was found great linearity of enramycin in each tissue, with a coefficient of variation above 0.99. Satisfactory recoveries from four different spiking levels were acquired (70.99-101.40%) while the relative standard deviations were all below 9%. The limit of quantification of enramycin in the present study is 5 μg/kg in fat and 10 μg/kg in other tissues, meeting the requirements for conducting the corresponding safety evaluation study. This method was demonstrated with excellent specificity, stability, and high sensitivity. To conclude, this novel approach is sufficiently sensitive and robust for the safety evaluation of enramycin in food products.
恩拉霉素是一种常用于鸡和猪的生长促进剂,对革兰氏阳性菌敏感,其设定的最大残留限量(MRL)为30μg/kg。然而,已报道的检测恩拉霉素的方法未能满足准确性要求,所需的定量限高于MRL。为解决这一问题,我们开发了一种基于超高效液相色谱-质谱联用(UHPLC-MS/MS)的高灵敏度且稳健的分析方法,用于测定猪组织(包括肝脏、肾脏、猪肉和脂肪)中的恩拉霉素残留。在使用含0.2M盐酸的55%甲醇混合物提取后,选择ENV柱对分析物进行净化和富集。经过全面验证,该方法在各组织中恩拉霉素的线性关系良好,相关系数均高于0.99。从四个不同加标水平获得了满意的回收率(70.99 - 101.40%),相对标准偏差均低于9%。本研究中恩拉霉素在脂肪中的定量限为5μg/kg,在其他组织中为10μg/kg,满足进行相应安全性评价研究的要求。该方法具有出色的特异性、稳定性和高灵敏度。总之,这种新方法对于食品中恩拉霉素的安全性评价具有足够的灵敏度和稳健性。