固相萃取/UPLC-MS/MS法检测饲料中18种喹诺酮类药物的研究

Determination of 18 Quinolones in Feeds with Solid Phase Extraction by UPLC-MS/MS

关键词:  超高效液相－串联质谱法  固相萃取  饲料  喹诺酮类药物

Key words:  UPLC-MS/MS  solid phase extraction  feeds  quinolones

摘要:

建立了超高效液相色谱色谱－串联串联质谱法测定饲料中18种喹诺酮类药物的分析方法。以0.1%乙酸乙腈提取饲料样品中的待测物，HLB柱净化，超高效液相色谱色谱－串联串联质谱法测定，氘代同位素内标法定量。18种喹诺酮类药物在线性范围为0～1.0 mg/L，线性关系良好，相关系数分别在0.9989~0.9999之间，方法的检测限为0.005 ~ 0.2 mg/kg。在不同饲料中添加浓度范围为0.1~ 5.0 mg/kg，平均回收率43.0% ~ 101%，相对标准偏差小于11.2%。实验证明，该方法灵敏、高效、抗干扰力强，适用于饲料中的18种喹诺酮类药物的测定。

Abstract:

An ultra high performance liquid chromatography - tandem mass spectrometry (UPLC－MS/MS) mehtod was developed to determine 18 quinolones in feeds. 18 quinolones were extracted by 0.1% acetic acid-acetonitrile solution , cleaned up with SPE of HLB column and detected by UPLC－MS/MS. Quantitative results were based by isotope internal standard method. The calibration curve of 18 quinolones showed good linearity in the range of 0~1.0 mg /L with conrrelation coefficient of 0.9989 and 0.9998 respectively. The detection limits of method were 0.005 ~ 0.2 mg /kg. The average recoveries of 18 quinolones at the spiked levels of 0.1 ~ 5.0 mg/kg in feeds ranged from 43.0 % ~ 101 % with relative standard deviation less than 11.2 %. Experiments showed that the method was sensitive, high efficiency and good anti-interference. The method adapted to the detection of 18 quinolones in feeds.