土壤中氟苯尼考及氟苯尼考胺高效液相色谱检测方法的研究

Determination of Florfenicol and Florfenicol Amine in Soil by High Performance Liquid Chromatography

关键词:  氟苯尼考  氟苯尼考胺  土壤  高效液相色谱法

Key words:  florfenicol  florfenicol amine  soil  HPLC method

摘要:

建立了土壤中氟苯尼考及氟苯尼考胺高效液相色谱（HPLC）检测方法。土壤样品采用超声提取法，提取试剂为丙酮和水，再与二氯甲烷进行液-液萃取净化杂质。用Agilent SB-C18色谱柱进行分离后用光电二极管阵列检测器检测，流动相为磷酸二氢钠溶液（0.01mol/L，含0.005mol/L十二烷基硫酸钠，pH=4.4）和乙腈（v:v=65:35）。在0.025~5mg/L浓度范围内，峰面积与浓度呈良好的线性关系，相关系数r均达0.999，氟苯尼考及氟苯尼考胺检测限分别为0.01mg/kg、0.015mg/kg，定量限分别为0.045mg/kg、0.05mg/kg。三种土壤中添加浓度为0.05mg/kg，0.1mg/kg，0.2mg/kg时，氟苯尼考和氟苯尼考胺标准工作液的回收率分别为90.16~99.37%、67.63~96.86%，日内变异系数均≤7.83%，日间变异系数均≤10.52%。该方法高效快速，操作简单，成本低，可用于氟苯尼考及氟苯尼考胺的同时检测。

Abstract:

This study established a high performance liquid chromatography (HPLC) detection methods for florfenicol and florfenicol amine in soil. The soil samples were extracted by ultrasonic method with acetone and water as extraction reagents, and then the impurities were purified by liquid-liquid extraction with dichloromethane. Using Agilent SB-C18 column for separation and detected by a photodiode array detector. The mobile phases were sodium dihydrogen phosphate solution(0.01mol/l, containing 0.005mol/l sodium dodecyl sulfate, pH = 4.4)and acetonitrile（v:v=65:35）. The method showed a good linear relationship between peak area and concertration at the range of 0.025~5mg/L, the correlation coefficient r all reached 0.999, the limit of detection florfenicol and florfenicol amine were 0.01mg/kg and 0.015mg/kg respectively, the limit of quantitation were 0.045mg/kg and 0.05mg/kg respectively. The recovery rate of florfenicol and florfenicol amine were 90.16~99.37% and 67.63~96.86% respectively, the intra-day CV ≤ 7.83%, and the inter-day CV ≤ 10.52%. This method was accurate, simple and cheap. It can be used for simultaneous determination of florfenicol and florfenicol amine in soil.