Determination of eight quinolones in milk using immunoaffinity microextraction in a packed syringe and liquid chromatography with fluorescence detection
Determination of eight quinolones in milk using immunoaffinity microextraction in a packed syringe and liquid chromatography with fluorescence detection
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使用包装注射器中的免疫亲和微萃取和荧光检测液相色谱法测定牛奶中的八种喹诺酮类药物
DOI：
10.1016/j.jchromb.2017.09.004
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发表时间：
2017
期刊：
影响因子：
--
通讯作者：
li cun
中科院分区：
文献类型：
--
作者：
zhang xinda;wang cuicui;yang linyan;zhang wei;lin jing;li cun
我们建立了一种新的、高选择性、灵敏的方法来测定牛奶中的八种喹诺酮类药物 (QN)：达诺沙星、恩诺沙星、奥比沙星、诺氟沙星、氧氟沙星、洛美沙星、氟罗沙星和环丙沙星。该方法使用填充注射器中的免疫亲和微萃取和荧光检测液相色谱 (IA-MEPS-LC-FLD)。传统上，QN 残留是通过液液萃取 (LLE) 和固相萃取 (SPE) 样品制备技术来测定；然而，这些方法非常耗时并且需要大量有机溶剂。因此，我们开发了一种结合 MEPS 的新型免疫亲和吸附剂，用于 QN 残留分析。使用戊二醛将0.2g与QN单克隆抗体结合的微珠填充到注射器中。本文对IA-MEPS方法的相关参数进行了优化和讨论。牛奶样品以3.5 mL/min的流速提取，用600 μL甲醇和磷酸盐缓冲盐水（9:1，v/v）洗脱，样品氮气干燥后用200 μL流动相复溶。然后，通过LC-FLD检测样品。对于八个 QN，检测限范围为 0.05 至 0.1 ng/g，定量限范围为 0.15 至 0.3 ng/g，日内和日间精密度分别为 3.2%–14.6% 和 9.1%–15.8%。 IA-MEPS方法的优点包括操作简单、成本低、减少有机溶剂的使用。此外，由于减少了溶剂体积要求，样品预处理是环保的。
We have established a new, highly selective, and sensitive method for the determination of eight quinolones (QNs) in milk: danofloxacin, enrofloxacin, orbifloxacin, norfloxacin, ofloxacin, lomefloxacin, fleroxacin, and ciprofloxacin. The method uses immunoaffinity microextraction in a packed syringe and liquid chromatography with fluorescence detection (IA-MEPS-LC-FLD). Traditionally, QN residues are determined by liquid–liquid extraction (LLE) and solid phase extraction (SPE) sample preparation techniques; however, these methods are timeconsuming and require large quantities of organic solvents. We thus developed a novel immunoaffinity adsorbent combined with MEPS for QN residue analysis. The syringe was filled with 0.2 g of microbeads bound with a QN monoclonal antibody using glutaraldehyde. The relevant parameters of the IA-MEPS method were optimized and discussed herein. Milk samples were extracted at a flow rate of 3.5 mL/min, 600 μL of methanoland phosphate-buffered saline (9:1, v/v) was used for elution, and 200 μL of mobile phase was used for reconstitution after the sample was dried with nitrogen. Then, the sample was detected by LC-FLD. For the eight QNs, the limit of detection ranged from 0.05 to 0.1 ng/g, the limit of quantification ranged from 0.15 to 0.3 ng/g, and the intra- and inter-day precision were 3.2%–14.6% and 9.1%–15.8%, respectively. The advantages of the IA-MEPS method includ simple operation, low cost and reduced organic solvent use. Moreover, the sample pretreatment is environmentally friendly because of the reduced solvent volume requirements.