Kośka Izabella, Purgat Krystian, Głowacki Rafał, Kubalczyk Paweł
Department of Environmental Chemistry, Faculty of Chemistry, University of Lodz, Pomorska 163, 90-236 Lodz, Poland.
Doctoral School of Exact and Natural Sciences, University of Lodz, Banacha 12/16, 90-237 Lodz, Poland.
Molecules. 2021 Nov 17;26(22):6931. doi: 10.3390/molecules26226931.
We have developed a precise and accurate method for the determination of ciprofloxacin and ofloxacin in meat tissues. Our method utilizes capillary electrophoresis with a transient pseudo-isotachophoresis mechanism and liquid-liquid extraction during sample preparation. For our experiment, a meat tissue sample was homogenized in pH 7.00 phosphate buffer at a ratio of 1:10 (tissue mass: buffer volume; g/mL). The extraction of each sample was carried out twice for 15 min with 600 µL of a mixture of dichloromethane and acetonitrile at a 2:1 volume ratio. We then conducted the electrophoretic separation at a voltage of 16 kV and a temperature of 25 °C using a background electrolyte of 0.1 mol/L phosphate-borate (pH 8.40). We used the UV detection at 288 nm. The experimentally determined LOQs for ciprofloxacin and ofloxacin were 0.27 ppm (0.8 nmol/g tissue) and 0.11 ppm (0.3 nmol/g tissue), respectively. The calibration curves exhibited linearity over the tested concentration range of 2 to 10 nmol/g tissue for both analytes. The relative standard deviation of the determination did not exceed 15%, and the recovery was in the range of 85-115%. We used the method to analyze various meat tissues for their ciprofloxacin and ofloxacin contents.
我们开发了一种精确且准确的方法来测定肉类组织中的环丙沙星和氧氟沙星。我们的方法在样品制备过程中利用了具有瞬态假等速电泳机制的毛细管电泳和液 - 液萃取。在我们的实验中，将肉类组织样品以1:10（组织质量：缓冲液体积；g/mL）的比例在pH 7.00的磷酸盐缓冲液中匀浆。每个样品用600 μL体积比为2:1的二氯甲烷和乙腈混合物进行两次15分钟的萃取。然后，我们使用0.1 mol/L磷酸盐 - 硼酸盐（pH 8.40）的背景电解质，在16 kV的电压和25 °C的温度下进行电泳分离。我们在288 nm处使用紫外检测。实验测定的环丙沙星和氧氟沙星的定量限分别为0.27 ppm（0.8 nmol/g组织）和0.11 ppm（0.3 nmol/g组织）。两种分析物的校准曲线在2至10 nmol/g组织的测试浓度范围内均呈线性。测定的相对标准偏差不超过15%，回收率在85 - 115%的范围内。我们使用该方法分析了各种肉类组织中的环丙沙星和氧氟沙星含量。
