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为了探索经济适用的氟喹诺酮类残留提取和检测方法,建立了同时测定牛奶中6种氟喹诺酮类药物残留的高效液相色谱(HPLC)串联荧光检测器(FLD)检测方法。样品经过含有5%乙酸的乙腈溶液涡旋提取,经改良Qu ECh ERS方法净化,HPLC-FLD检测,激发波长280 nm,发射波长450 nm,色谱柱为Waters XBridgeTM-C18柱(4.6 mm×250 mm,5μm),流速1.0 m L/min,柱温30℃,以乙腈和含0.1%甲酸的20 mmol/L甲酸铵水溶液做为流动相进行梯度洗脱。在所建立的方法中6种氟喹诺酮分离度较好(R>1.5),在0.01~0.3μg/m L浓度范围内具有良好的关系(r=0.999 9),检出限在0.97~3.91μg/kg之间,回收率试验中平均加标回收率为97%~100%;重复性、精密度、稳定性试验结果良好,相对标准偏差均<3%。所建立方法简单、快速、灵敏度和回收率高,适用于牛奶中该6种氟喹诺酮类药物残留的大批量筛选和定量测定。
In order to explore an economical method for the extraction and detection of fluoroquinolones residue, a high performance liquid chromatography (HPLC) tandem fluorescence detector (FLD) detection method was developed for the simultaneous determination of six fluoroquinolones residues in milk. The sample was vortexed with acetonitrile containing 5% acetic acid and purified by a modified Qu ECh ERS method with HPLC-FLD. The excitation wavelength was 280 nm and the emission wavelength was 450 nm. The column was a Waters XBridgeTM-C18 column (4.6 mm × 250 mm , 5μm) at a flow rate of 1.0 m L / min. The column temperature was 30 ℃. The mobile phase consisted of acetonitrile and 0.1% formic acid in 20 mmol / L aqueous ammonium formate. In the established method, the separation of the six fluoroquinolones was good (R> 1.5), with a good correlation (r = 0.999 9) at a concentration range of 0.01-0.3 μg / mL with a detection limit of 0.97-3.91 μg / kg, the recoveries were average recovery of 97% to 100%; repeatability, precision, stability test results were good, the relative standard deviation were <3%. The established method is simple, rapid, high sensitivity and recovery, suitable for large-scale screening and quantitative determination of the six fluoroquinolone residues in milk.