Zhao Ying, Liu Yu, Jin Yan, Xu Yihong, Zhong Yu, Jiang Shi, Li Xiaodong, Zeng Fan, Zhou Jiannan
Shenyang Entry-Exist Inspection and Quarantine Bureau, Shenyang 110016, China.
Se Pu. 2012 Sep;30(9):908-14. doi: 10.3724/sp.j.1123.2012.06019.
An ultra performance liquid chromatography with electrospray ionization tandem mass spectrometry (UPLC-ESI-MS/MS) method was developed for the simultaneous determination of 29 veterinary drugs of quinolones, sulfonamides, macrolides and nitrofurans in compound feeds. The sample was extracted with methanol-acetonitrile ( 1 : 1, v/v), and then cleaned up using solid phase extraction with an Oasis HLB column, detected by UPLC-ESI-MS/ MS. The UPLC separation was performed on a C18 column (100 mm x 2.1 mm, 1.7 microm) using a gradient elution with the mobile phases of methanol and 0. 1% (v/v) formic acid aqueous solution. The ESI-MS/MS detection was achieved in positive mode under multiple reaction monitoring (MRM) mode. The linear ranges were from 0.01 to 5.0 mg/L with the correlation coefficients above 0. 99 for all the 29 veterinary drugs. The average recoveries of the 29 veterinary drugs spiked in three feed matrixes (the compound premix feed, the complete formula feed and the concentrated feed) at four spiked levels were 61.2% - 94.3% with the relative standard deviations (RSDs) of 2.2% - 15.0%. The limits of detection were 0. 01 mg/kg or 0.05 mg/kg. The method is rapid, accurate, reproducible, sensitive and easy to apply, and suitable for the simultaneous determination of diverse veterinary drugs in compound feeds.
建立了一种超高效液相色谱-电喷雾电离串联质谱(UPLC-ESI-MS/MS)法,用于同时测定复合饲料中喹诺酮类、磺胺类、大环内酯类和硝基呋喃类29种兽药。样品用甲醇-乙腈(1:1,v/v)提取,然后用Oasis HLB柱进行固相萃取净化,采用UPLC-ESI-MS/MS检测。UPLC分离在C18柱(100 mm×2.1 mm,1.7μm)上进行,以甲醇和0.1%(v/v)甲酸水溶液为流动相进行梯度洗脱。ESI-MS/MS检测在正离子模式下的多反应监测(MRM)模式下进行。29种兽药的线性范围为0.01~5.0 mg/L,相关系数均大于0.99。在三种饲料基质(复合预混料、全价配合饲料和浓缩饲料)中添加29种兽药,在四个添加水平下的平均回收率为61.2%~94.3%,相对标准偏差(RSD)为2.2%~15.0%。检测限为0.01 mg/kg或0.05 mg/kg。该方法快速、准确、重现性好、灵敏度高且易于应用,适用于同时测定复合饲料中多种兽药。