液相色谱-串联质谱法检测中兽药中非法添加氟喹诺酮类药物含量的不确定度评估

Uncertainty evaluation of fluoroquinolones illegally added in veterinary herbal medicine by liquid chromatography-tandem mass spectrometry

目的评估液相色谱-串联质谱法检测中兽药中非法添加氟喹诺酮类药物含量的不确定度。方法建立液相色谱-串联质谱法检测中兽药(肥猪散、健胃散、银翘散)中非法添加氟喹诺酮类药物的含量测定方法,根据JJF1059.1-2012《测量不确定度评定与表示》的相关规定,对该方法的不确定度进行评定。结果中兽药中氟喹诺酮类药物含量分别为C(Enro)=100.90mg/kg、C(Cip)=100.34mg/kg、C(Norf)=100.21mg/kg、C(Oflo)=100.61mg/kg时,95%置信水平下,取k=2,不确定度评估结果分别表示为X(Enro)=(100.90±6.957)mg/kg;X(Cip)=(100.34±7.067)mg/kg;X(Norf)=(100.21±6.898)mg/kg;X(Oflo)=(100.61±6.957)mg/kg。结论评定结果表明,影响检测结果的主要因素为液相色谱-串联质谱仪的灵敏度、天平的精密度、操作的规范性。

Objective To evaluate the uncertainty of determination of fluoroquinolones illegally added in veterinary medicine by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Methods A method for the determination of fluoroquinolones illegally added in veterinary herbal medicine (feizhu powder, Jianwei powder, Yinqiao powder) by liquid chromatography-tandem mass spectrometry was established. According to the relevant provisions of JJF1059.1-2012 Measurement uncertainty evaluation and representation, the uncertainty of the method was evaluated. Results The content of fluoroquinolones in veterinary medicine was C(Enro)=100.90 mg/kg, C(Cip)=100.34 mg/kg, C(Norf)=100.21 mg/kg, C(Oflo)=100.61 mg/kg, respectively, when 95% confidence level, k=2, and the evaluation results were X(Enro)=(100.90±6.957) mg/kg, X(Cip)=(100.34±7.067) mg/kg, X(Norf)=(100.21±6.898) mg/kg, X(Oflo)=(100.61±6.957) mg/kg, respectively. Conclusion The main sources of uncertainty are the sensitivity of the liquid chromatography-tandem mass spectrometer, the precision of the balance, and the standard of operation.