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首页> 外文会议>Πανελληνιο Συνεδριο ΤροΦιμων >DEVELOPMENT AND VALIDATION OF A LIQUID CHROMATOGRAPHY - MASS SPECTROMETRIC METHOD FOR THE DETERMINATION OF SULFADIAZINE IN FISH MUSCLE
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DEVELOPMENT AND VALIDATION OF A LIQUID CHROMATOGRAPHY - MASS SPECTROMETRIC METHOD FOR THE DETERMINATION OF SULFADIAZINE IN FISH MUSCLE

机译：液相色谱-质谱法测定鱼肉中磺胺二氮的研制与验证。

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Sulfadiazine (SDZ) belongs to antibacterial agents used in fish-farm. Several methods have been developed for the determination of SDZ in fish tissues because of the increasing concern for consumers protection from drug residues. In this study a method by Liquid Chromatography - Mass Spectrometry for the determination of SDZ in muscle tissue of the cultured fish gilthead sea bream (Sparus aurata) and gilthead sea bass (Dicentrarchus labrax) is developed and validated, using dapsone (DPS) as internal standard. Sulfadiazine is extracted by Accelerated Solvent Extractor (ASE) using water as extraction solvent. Optimized extraction conditions are: temperature 100 °C, pressure 1500 psi, static time 15 min, cell size 11 mL, 1 extraction cycle, flush volume 60 %. The ASE extract is diluted to 20 mL, then is cooled and centrifuged. A portion of 4 mL is loaded onto a Nexus (60mg/3mL) SPE cartridge, which has been conditioned with 2 mL methanol and 2 mL water. The cartridge is washed with 4 mL of mixture methanol/water 5/95 (v/v). The cartridge is dried and sulfadiazine is eluted with 2 mL methanol. The mixture is dried and reconstituted with 0.2 mL of water/acetonitrile mixture 90/10 (v/v). The chromatographic analysis was performed using an HPLC system model Alliance 2695 (Waters, USA). An XTerra MS C18 2.1x100 mm, 3.5 nm analytical column was used (Waters, USA). Separation was performed at a column temperature of 40 °C with a mobile phase flow rate of 0.2 mLmin~(-1). Mobile phase was consisted of solvent A (water containing formic acid 0.05 %) and solvent B (acetonitrile containing formic acid 0.05 %) and a gradient elution programme was applied. Initially 90 % of solvent A was reduced to 2 % in the first ten minutes. In the next half of minute is increased to 98 % and maintained for the next six minutes. Injection volume was 5 μL. A ZQ-2000 Micromass mass spectrometer with the MassLynx software (Waters, USA), was operated in positive ESI mode measuring 251 m/z ion for SDZ and 249 m/z ion for DPS. Optimized conditions for MS were: capillary voltage 3.0 kV, cone voltage 20 V, source temperature 120 °C. The method was validated for major analytical characteristics. A calibration curve was found linear in the concentration range 9-150 ngmL~(-1). The Limit of Detection was found 3 μgkg~(-1) and the Limit of Quantification was 9 μgkg~(-1). Method mean Recovery achieved was 90.0±3.6 (mean ± SD) for blank fortified samples (n=6) range at 50,100 and 150 μgkg~(-1). The method is suitable for fast and accurate determination of SDZ residues in cultured sea bream and sea bass.
机译：磺胺嘧啶（SDZ）属于鱼类养殖场中使用的抗菌剂。由于越来越多地关注消费者对药物残留的保护，因此已经开发出了几种测定鱼组织中SDZ的方法。在这项研究中，采用氨苯砜（DPS）作为内部溶液，通过液相色谱-质谱法测定并验证了养殖鱼fish头鲷（Sparus aurata）和and头鲈（Dicentrarchus labrax）肌肉组织中SDZ的测定方法。标准。磺胺嘧啶通过加速溶剂萃取器（ASE）以水为萃取溶剂进行萃取。优化的萃取条件为：温度100°C，压力1500 psi，静态时间15分钟，样品池大小11 mL，萃取周期1次，冲洗量60％。 ASE萃取液稀释至20 mL，然后冷却并离心。将部分4 mL装入Nexus（60mg / 3mL）SPE柱上，该柱已用2 mL甲醇和2 mL水调节。用4mL甲醇/水5/95（v / v）的混合物洗涤该柱。干燥柱，用2mL甲醇洗脱磺胺嘧啶。将混合物干燥并用0.2mL水/乙腈混合物90/10（v / v）重构。色谱分析使用HPLC系统型号Alliance 2695（Waters，USA）进行。使用XTerra MS C18 2.1x100 mm，3.5 nm分析柱（沃特世，美国）。分离在40°C的柱温下进行，流动相流速为0.2 mLmin〜（-1）。流动相由溶剂A（含有0.05％的甲酸的水）和溶剂B（含有0.05％的甲酸的乙腈）组成，并应用了梯度洗脱程序。在最初的十分钟内，最初将90％的溶剂A还原为2％。在接下来的半分钟内，将增加到98％，并在接下来的六分钟内进行维护。进样量为5μL。使用MassLynx软件（美国沃特世）的ZQ-2000微质谱仪在正ESI模式下运行，测量SDZ为251 m / z离子，DPS为249 m / z离子。 MS的最佳条件是：毛细管电压3.0 kV，锥电压20 V，源温度120°C。验证了该方法的主要分析特性。发现校准曲线在9-150 ngmL〜（-1）的浓度范围内呈线性关系。检出限为3μgkg〜（-1），定量限为9μgkg〜（-1）。在50,100和150μgkg〜（-1）范围内，空白强化样品（n = 6）的方法平均回收率达到90.0±3.6（平均值±SD）。该方法适用于快速准确地测定养殖鲷鱼和鲈鱼中SDZ残留量。

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