摘要

采用细胞内清除法与超高效液相色谱 - 串联质谱法（UPLC-MS / MS）联用开发了一种加速溶剂萃取（ASE），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种霉酚酸类药物，2种β-内酰胺类药物，1种林肯酰胺和甲氧苄啶。采用2g C18作吸附剂，在80℃，1个静态循环5min，用甲醇/乙腈（1/1，v / v）获得ASE方法的最佳参数。在RSD低于20％的情况下，回收率达到50.1-129.2％。方法检测限为0.03至2.9μgkg-1。与报道的超声辅助提取法相比，所提出的方法提供了对来自海参的磺酰胺类似的提取效率，但对于其他类别的抗生素提供了更高的提取效率。该验证方法成功应用于海参样品中，诺氟沙星检测出9种抗生素，最高检测浓度可达57.7μg kg^-1。

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.

https://www.sciencedirect.com/science/article/pii/S0308814618304837