基质工作曲线法和标准加入法测定鸡肝粉中的环丙沙星

Comparison of matrix working curve method and standard addition method for the determination of ciprofloxacin in chicken liver powder

建立了鸡肝粉中环丙沙星的超高效液相色谱/串联质谱检测方法。鸡肝粉样品中加入环丙沙星-d8后用二次水溶解,再经甲酸-乙腈溶液提取,用乙腈饱和的正己烷液液分配净化,浓缩定容后采用正离子多反应监测模式分析,基质工作曲线法定量。在0.02,0.2,1.0 mg/kg 3个添加水平下进行验证实验,方法的线性范围为1~100 ng/m L,平均回收率为96.5%~100.7%,相对标准偏差为1.3%~10.2%。分别利用基质工作曲线法和标准加入法对两份鸡肝粉质控样品进行定量。结果表明,两种方法所得数值均为说明书要求的满意结果,但是后者更接近于指定值。因此,在方法灵敏度允许的情况下,采用标准加入法分析阳性样品更有利于获得准确的结果。

A method was developed for the determination of ciprofloxacin in chicken liver powder based on ultra performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry（UPLC-ESI-MS/MS）.Ciprofloxacin-d8 was added into the chicken liver powder.Then the samples were extracted with water and formic acid-acetonitrile.Hexane saturated with acetonitrile was used for cleanup.The eluate was dried and redissolved in acetonitrile-0.1% formic acid（1：9,V/V）,then quantified by UPLC – ESI – MS/MS operated in positive multiple-reaction mode（MRM）.The matrix-matched internal standard calibration curves were used for quantitative determination.The linear range was from 1 to100 ng/mL.The average recoveries were from 96.5% to 100.7% with the relative standard deviations of1.3% - 10.2% at 0.02,0.2,1.0 mg/kg.The limit of detection（LOD） was 0.006 mg/kg and the limit of quantification（LOQ） was 0.02 mg/kg.LOD and LOQ were 0.05 mg/kg and 0.17 mg/kg respectively using standard addition method.In the end,matrix working curve method and standard addition method were used to determine ciprofloxacin in two quality control samples.It showed that all the results were satisfactory according to instruction,but the one obtained by the latter was closer to the given values.So standard addition method is advantageous to analyze positve samples if the sensitivity of this methad allows.