采用细胞内净化加速溶剂萃取与超高效液相色谱-串联质谱联用测定海参中的 21 种抗生素。
Determination of 21 antibiotics in sea cucumber using accelerated solvent extraction with in-cell clean-up coupled to ultra-performance liquid chromatography-tandem mass spectrometry.
机构信息
Key Laboratory of Industrial Ecology and Environmental Engineering (MOE), School of Environmental Science and Technology, Dalian University of Technology, Dalian 116024, China.
Key Laboratory of Industrial Ecology and Environmental Engineering (MOE), School of Environmental Science and Technology, Dalian University of Technology, Dalian 116024, China.
出版信息
Food Chem. 2018 Aug 30;258:87-94. doi: 10.1016/j.foodchem.2018.03.051. Epub 2018 Mar 14.
An accelerated solvent extraction (ASE) with in-cell clean-up method coupled to ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed to determine 21 antibiotics in sea cucumber. The analytes include 10 sulfonamides, 4 fluoroquinolones, 3 amphenicols, 2 beta-lactams, 1 lincosamide and trimethoprim. Optimal parameters of ASE method were obtained at 80 °C, 1 static cycle of 5 min with methanol/acetonitrile (1/1, v/v) using 2 g of C18 as adsorbent. Recoveries at 50.1-129.2% were achieved with RSD under 20%. Method detection limits ranged from 0.03 to 2.9 μg kg. Compared to the reported ultrasound-assisted extraction method, the proposed method offered comparable extraction efficiency for sulfonamides from sea cucumber, but higher for other categories of antibiotics. This validated method was then successfully applied to sea cucumber samples and 9 antibiotics were detected with the highest concentration up to 57.7 μg kg for norfloxacin.
建立了一种加速溶剂萃取（ASE）与细胞内净化方法相结合的超高效液相色谱-串联质谱（UPLC-MS/MS）方法，用于测定海参中的 21 种抗生素。分析物包括 10 种磺胺类药物、4 种氟喹诺酮类药物、3 种酰胺醇类药物、2 种β-内酰胺类药物、1 种林可酰胺类药物和 1 种甲氧苄啶。在 ASE 方法中，最佳参数为 80°C，1 个静态循环 5min，使用 2g C18 作为吸附剂，甲醇/乙腈（1/1，v/v）。回收率在 50.1-129.2%之间，RSD 低于 20%。方法检测限范围为 0.03-2.9μg/kg。与已报道的超声辅助提取方法相比，该方法对海参中磺胺类药物的提取效率相当，但对其他类别的抗生素的提取效率更高。该方法经过验证后成功应用于海参样品的检测，其中诺氟沙星的浓度最高可达 57.7μg/kg。
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