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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
Food Chemistry ( IF 8.5 ) Pub Date : 2018-03-14 , DOI: 10.1016/j.foodchem.2018.03.051
Minghua Zhu , Hongxia Zhao , Deming Xia , Juan Du , Huaijun Xie , Jingwen Chen

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−1. 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−1 for norfloxacin.



中文翻译:

加速溶剂萃取-池内净化-超高效液相色谱-串联质谱法测定海参中的21种抗生素

结合细胞内净化方法和超高效液相色谱-串联质谱(UPLC-MS / MS)的加速溶剂萃取(ASE)技术开发,用于测定海参中的21种抗生素。分析物包括10种磺酰胺,4种氟喹诺酮,3种苯甲酚,2种β-内酰胺,1种林可酰胺和甲氧苄啶。ASE方法的最佳参数是在80°C,使用2 g C18作为吸附剂的甲醇/乙腈(1/1,v / v)的1个静态循环5分钟下获得的。RSD低于20%时,回收率为50.1–129.2%。方法检测极限范围为0.03至2.9μgkg -1。与报道的超声辅助提取方法相比,该方法对海参中的磺胺类药物提供了可比的提取效率,但对其他种类的抗生素却具有更高的提取效率。然后将该验证方法成功地应用于海参样品,并检测出9种抗生素,诺氟沙星的最高浓度最高可达57.7μgkg -1

更新日期:2018-03-14
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