摘要
建立了固相萃取净化/超高效液相色谱-串联质谱同时测定猪肉中14种大环内酯类药物残留的方法。样品经70%(体积分数)乙腈提取,固相萃取柱(HLB柱)富集净化后,使用BEHC18色谱柱(100mm×2.1mm,1.7μm)分离,以乙腈和0.1%甲酸-2mmol/L乙酸铵溶液为流动相进行梯度洗脱。在正离子模式下,采用多反应监测模式分段扫描,外标法定量。结果表明,14种大环内酯类药物在对应质量浓度范围内均呈良好的线性关系,相关系数(r^2)均大于0.995,方法检出限为0.1~0.8μg/kg,定量下限为0.5~3.0μg/kg,在低、中、高3个加标水平下的回收率为71.1%~102%,相对标准偏差(RSD)均小于6.0%。该方法准确、可靠,可用于猪肉中大环内酯类药物的检测。
An ultra performance liquid chromatography-tandem mass spectrometric method with solid phase extraction was established for the simultaneous determination of 14 macrolide drugs in pork samples.Samples were extracted with 70%(volume fraction)acetonitrile,purified by solid phase extraction using a hydrophilic-lipophilic balanced(HLB)polymer,and separated on a C18 column(100 mm×2.1 mm,1.7μm)with acetonitrile and 0.1%formic acid-2 mmol/L ammonium acetate solution as mobile phases by gradient elution.The analytes were detected by mass spectrometry in positive ion mode under multiple reaction monitoring(MRM)scanning mode,and quantified by external standard method.Results showed that good linearities for 14 macrolide drugs were obtained in the corresponding mass concentration ranges with correlation coefficients(r^2)larger than 0.995.The detection limits and quantitation limits of the method were in the ranges of 0.1-0.8μg/kg and 0.5-3.0μg/kg,respectively.Recoveries at low,medium and high spiked levels were in the range of 71.1%-102%,with relative standard deviations(RSD)less than 6.0%.This method could be applied in the analysis of macrolide drugs in pork samples with good accuracy and reliability.
作者
王一涵
王展华
陈万勤
王峰
刘柱
WANG Yi-han;WANG Zhan-hua;CHEN Wan-qin;WANG Feng;LIU Zhu(Zhejiang Institute for Food and Drug Control,Hangzhou 310052,China)
出处
《分析测试学报》
CAS
CSCD
北大核心
2019年第10期1247-1253,共7页
Journal of Instrumental Analysis
基金
浙江省公益性项目(LGF18C200001)
关键词
固相萃取
超高效液相色谱-串联质谱法
大环内酯类药物
猪肉
solid phase extraction
ultra performance liquid chromatography-tandem mass spectrometry
macrolide drugs
pork
