液相色谱-质谱/质谱法测定牛乳中庆大霉素  

Determination of Gentamycin in Milk by HPLC-MS/MS

作　　者：程艳宇[1] 张金环[1] 刘正[1] 闫磊[1] Cheng Yanyu;Zhang Jinhuan;Liu Zheng;Yan Lei(Tianjin Dairy and Food Monitoring Center,Tianjin 300381,China)

机构地区：[1]天津市乳品食品监测中心,天津300381

出　　处：《现代食品》2020年第14期176-181,195,共7页Modern Food

摘　　要：建立了一种不使用离子对试剂测定牛奶样品中庆大霉素的液相色谱-质谱/质谱检验方法。样品经三氯乙酸溶液提取,然后在MCX固相萃取柱净化,使用HPLC-MS/MS多反应监测(MRM)模式进行定性、定量分析,净化液在高效液相色谱柱上以0.1%甲酸水溶液和乙腈为流动相进行梯度洗脱分离,质谱采集模式为电喷雾正离子监测模式。结果表明,庆大霉素各组分C1、C2+C2a、C1a在10~1000、20~2000、10~1000 ng·mL^-1范围内,峰面积与浓度线性良好,相关系数均>0.99;方法的检出限(LOD)分别为2.0、4.0、2.0μg·kg^-1,平均加标回收率达到63.2%~90.3%。该方法取消了传统方法的离子对试剂的使用,操作简便,满足对庆大霉素的定性和定量的要求,避免了离子对试剂对质谱的潜在影响。A method was established for the determination of gentamicin in milk samples by HPLC-MS/MS without using ion pair reagents.The sample was extracted by trichloroacetic acid solution,followed by MCX solidphase extraction(SPE)as the cleanup procedure.High Performance Liquid Chromatography-Mass Spectrometry/Mass Spectrometry(HPLC-MS/MS)was used for identification and quantification of antibiotics.The separation was carried out on a CAPCELL PAK ST column with a gradient elution using 0.1%formic acid and acetonitrile.The mass spectrometer was operated in the positive ion mode using multiple reaction ion monitoring(MRM)mode.The results showed that in the range of 10~1000,20~2000 and 10~1000 ng·ml^-1,the peak area and concentration of gentamicin components C1,C2+C2a and C1a have good linearity,and the correlation coefficient is>0.99;The LOD is 2.0,4.0 and 2.0μg·kg^-1 and the average recovery is 63.2%~90.3%.The method canceled the use of traditional ion pair reagents,which could protect the mass spectrometer avoiding contaminating.It is simple to operate and meets the qualitative and quantitative requirements of gentamicin.

关 键 词：氨基糖苷 庆大霉素 固相萃取 液相色谱-质谱/质谱法 离子对试剂 

分 类 号：R917[医药卫生—药物分析学]