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采用加压液相萃取和液相色谱-串联质谱法对火锅底料中的甾体激素和抗生素进行多类测定。

Multi-class determination of steroid hormones and antibiotics in fatty hotpot ingredients by pressurized liquid extraction and liquid chromatography-tandem mass spectrometry.

机构信息

School of Pharmacy, Shenyang Pharmaceutical University, 103 Wenhua Road Shenhe District, 110016, Shenyang, Liaoning Province, PR China.

School of Pharmacy, Shenyang Pharmaceutical University, 103 Wenhua Road Shenhe District, 110016, Shenyang, Liaoning Province, PR China.

出版信息

J Pharm Biomed Anal. 2019 Jul 15;171:193-203. doi: 10.1016/j.jpba.2019.04.019. Epub 2019 Apr 15.

Abstract

Due to the misuse of hormones and antibiotics resulting in drug residues in meat products, serious concerns have arisen regarding to the potential risks for human health. In this paper, a simple and efficient method was developed to simultaneously quantify six steroid hormones and six antibiotics in fatty foods by combining pressurized liquid extraction (PLE) with ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). Adsorbents, extraction temperature, extraction time, recycle time and several other parameters were optimized in current investigation. The optimized PLE method was employed by using n-hexane-methanol-acetonitrile (2:1:1, v/v/v) as extraction solvent, silica gel as lipid sorbent, and the optimum parameters were 60 °C, 1500 psi and 10 min, respectively. Under the optimal conditions, the recoveries of spiked samples ranged from 82.2% to 115.0%. The limits of quantifications (LODs) were from 0.4 to 25.0 μg/kg. The developed PLE method was successfully applied to analyze steroid hormones and antibiotics in 27 fatty foods of hotpot ingredients without any additional clean-up steps. The results showed that the residues of estradiol benzoate (EB) and enrofloxacin (EN) in some matrices were much higher than maximum residue limits (MRLs) value, especially EB in fish, which exceeded 176.7 μg/kg. The results demonstrated that the developed method was sensitive and efficient in testing hotpot ingredients, and was an excellent analytical tool for monitoring residues of steroid hormones and antibiotics in fatty foods.

摘要

由于激素和抗生素的滥用导致肉品中药物残留,严重关切人类健康所面临的潜在风险。在本文中,开发了一种简单高效的方法,通过加压液体萃取(PLE)与超高效液相色谱-串联质谱(UHPLC-MS/MS)相结合,同时定量测定脂肪食品中的六种甾体激素和六种抗生素。在当前的研究中,对吸附剂、提取温度、提取时间、循环时间等几个参数进行了优化。采用正己烷-甲醇-乙腈(2:1:1,v/v/v)作为提取溶剂、硅胶作为脂溶性吸附剂、优化后的PLE 方法,优化后的提取温度为 60°C,提取压力为 1500psi,提取时间为 10min。在最佳条件下,加标样品的回收率为 82.2%至 115.0%。定量限(LOD)为 0.4 至 25.0μg/kg。该 PLE 方法成功地应用于火锅配料 27 种脂肪食品中甾体激素和抗生素的分析,无需进一步净化步骤。结果表明,一些基质中苯甲酸雌二醇(EB)和恩诺沙星(EN)的残留量远高于最大残留限量(MRL)值,特别是鱼中 EB 的残留量超过 176.7μg/kg。结果表明,该方法对检测火锅配料敏感高效,是监测脂肪食品中甾体激素和抗生素残留的有效分析工具。

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