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[固相萃取-高效液相色谱法同时测定牛组织中乙酰马啉和氯异美啶残留量]

[Simultaneous determination of diminazene aceturate and isometamidium chloride residues in cattle tissues by high performance liquid chromatography with solid-phase extraction].

作者信息

Zhou Yuhui, Zeng Zhenling, Yu Jingxian, Liu Rong, Pan Lihua, Zhong Qiuyu, Chen Hong

机构信息

College of Veterinary Medicine, South China Agricultural University, National Reference Laboratory of Veterinary Drug Residues, Guangzhou 510642, China.

出版信息

Se Pu. 2017 Sep 8;35(9):995-1002. doi: 10.3724/SP.J.1123.2017.04033.

Abstract

A method for the simultaneous determination of trypanocidal diminazene aceturate (DIM) and isometamidium chloride (ISM) that containing benzamidine groups in cattle tissues was developed by high performance liquid chromatography (HPLC) with solid-phase extraction (SPE). The tissue samples were extracted with different proportions of water-acetonitrile, then were cleaned up by Oasis WCX cartridges. DIM and ISM were separated by HPLC with a Spherisorb CN column (250 mm×4.6 mm, 5 μm). Acetonitrile-0.05 mol/L ammonium formate solution (pH 2.4) was used as mobile phases with gradient elution. The detection wavelength of UV was set at 380 nm. The limits of detection (LODs) and the limits of quantification (LOQs) of DIM and ISM in cattle tissues were 0.01 mg/kg and 0.025 mg/kg, respectively. The correlation coefficients () of DIM and ISM in cattle tissues were not less than 0.9993. The average recoveries of DIM and ISM at three spiked levels were 82.2%-97.6% with the intra-day relative standard derivations (RSDs) of 0.3%-5.2% (=5) and inter-day RSDs of 1.3%-5.2% (=15). The method was successfully applied to the analysis of DIM and ISM in cattle tissues. The method is rapid, sensitive and repeatable for the determination of diminazene aceturate and isometamidium chloride in cattle tissues.

摘要

建立了一种采用高效液相色谱(HPLC)结合固相萃取(SPE)同时测定牛组织中含苯甲脒基团的杀锥虫药乙酰氨基阿维菌素(DIM)和氯异美汀(ISM)的方法。组织样品用不同比例的水 - 乙腈提取,然后用Oasis WCX柱净化。DIM和ISM用Spherisorb CN柱(250 mm×4.6 mm,5μm)通过HPLC分离。乙腈 - 0.05 mol/L甲酸铵溶液(pH 2.4)用作流动相进行梯度洗脱。紫外检测波长设定为380 nm。牛组织中DIM和ISM的检测限(LOD)和定量限(LOQ)分别为0.01 mg/kg和0.01 mg/kg。牛组织中DIM和ISM的相关系数()不小于0.9993。DIM和ISM在三个加标水平下的平均回收率为82.2% - 97.6%,日内相对标准偏差(RSD)为0.3% - 5.2%(n = 5),日间RSD为1.3% - 5.2%(n = 15)。该方法成功应用于牛组织中DIM和ISM的分析。该方法用于测定牛组织中乙酰氨基阿维菌素和氯异美汀快速、灵敏且可重复。

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