摘要
建立了虾中万古霉素和去甲万古霉素残留量的高效液相色谱-串联质谱(HPLC-MS/MS)检测方法。样品经0.1%甲酸-乙腈(9∶1,体积比)混合溶液提取,乙腈饱和的正己烷除脂,PCX结合Florisil固相萃取柱进行净化后,以乙腈和0.1%甲酸溶液为流动相,经CAPCELL PAK MG-C18色谱柱分离后,采用高效液相色谱-串联质谱在多反应离子监测(MRM)模式进行测定,以双去氯万古霉素作为内标物,内标法定量。结果表明:万古霉素和去甲万古霉素在2~250 ng/m L范围内呈良好的线性关系,相关系数(r2)均大于0.99。在5,25,50μg/kg加标水平下,万古霉素和去甲万古霉素的平均回收率为87.2%~102%,相对标准偏差为1.3%~8.7%。方法的检出限(LOD)为2.0μg/kg,定量下限(LOQ)为5.0μg/kg。该方法灵敏、准确,重复性好,适用于虾类中万古霉素及去甲万古霉素残留量的测定。
A new method for the determination of vancomycin and norvancomycin residues in shrimps by high performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS） was established.Samples were extracted with 0.1% formic acid-acetonitrile solution,defatted with n hexane saturated with acetonitrile and purified with PCX and Florisil solid phase extraction column.The separation of two targets was carried out on a CAPCELL PAK MG-C18 column by gradient elution with 0.1% formic acid-acetonitrile as mobile phase.The identification of two analytes was performed in multi-reaction monitoring（MRM）,and the quantification was carried out by the internal standard method.Dedichloro vancomycin was used as an internal standard.The calibration curves showed good linearities in the range of 2-250 ng/mL with correlation coefficients（r2） greater than 0.99.The detection limits（LOD） of this method were both 2.0 μg/kg,and the limits of quantitation（LOQ） were 5.0 μg/kg.The recoveries of the target compounds at spiked levels of 5,25,50 μg/kg were in the range of 87.2%-102%,with relative standard deviations（RSDs） of 1.3%-8.7%.The results indicated that this method had high sensitivity,accuracy and good reproducibility.It was suitable for the simultaneous determination of ancomycin and norvancomycin residues in shrimps.
出处
《分析测试学报》
CAS
CSCD
北大核心
2017年第6期773-777,共5页
Journal of Instrumental Analysis
基金
农业行业标准制定和修定农产品质量安全项目(2130109)
