超高效液相色谱串联质谱法测定豆芽中恩诺沙星、环丙沙星残留量的不确定度评定

Evaluation of uncertainty in determination of enrofloxacin and ciprofloxacin residues in bean sprouts by ultra performance liquid chromatography-tandem mass spectrometry

利用超高效液相色谱—串联质谱法测定豆芽中恩诺沙星、环丙沙星的残留量,并根据建立的数学模型评定该方法的不确定度的各分量。样品用0.1%甲酸—乙腈提取,经prime HLB固相小柱净化,超高效液相色谱—串联质谱测定,内标法定量。评定结果表明,标准曲线拟合和标准溶液配置所产生的的不确定度分量最大。当豆芽中恩诺沙星含量为8.6μg/kg时,其扩展不确定度为1.5μg/kg(k=2),环丙沙星含量为11.0μg/kg时,其扩展不确定度为2.3μg/kg(k=2)。

A method for the determination of trace-enrofloxacin and ciprofloxacin in bean sprouts by using ultra-performance liquid chromatography-tandem mass spectrometry was established.The mathematical model was established and used to evaluate the uncertainty components of this method.The sample was extracted with 0.1%acid acetonitrile directly,and purified by prime HLB(SPE),then analyzed by UPLC-MS/MS.The results showed that the main sources of uncertainty arose from the standard curve fitting and standard solution.The expanded uncertainty was 1.5 and 2.3μg/kg for enrofloxacin and ciprofloxacin contents of 8.6 and 11.0μg/kg in bean sprouts(k=2),respectively.