液质联用法快速测定饲料中维吉尼亚霉素含量  

A Rapid Method for the Determination of Virginiamycin in Feeds Using Liquid Chromatographytandem Mass Spectrometry

作　　者：曹文卿[1,2] 吴振兴[2] 静平[2] 杨桂朋[1] 林黎明[2] 

机构地区：[1]中国海洋大学化学化工学院,山东青岛266100 [2]山东出入境检验检疫局检验检疫技术中心,山东青岛266002

出　　处：《食品研究与开发》2015年第12期79-83,共5页Food Research and Development

基　　金：国家自然科学基金重点项目(NO.41030858);国家自然科学基金创新研究群体项目(NO.41221004)

摘　　要：建立了饲料中快速测定维吉尼亚霉素M_1和S_1残留量的高效液相色谱-质谱/质谱(HPLC-MS/MS)方法。样品采用乙腈提取,经冷冻脱脂和饱和氯化钠溶液盐析净化,用甲醇-甲酸铵溶液定容,经SDB-C8色谱柱分离后,采用多反应监测(MRM)正离子模式检测,监测离子对分别为M1:m/z 526.3/355.1和526.3/337.2;S1:824.5/290.1和824.5/205.1。其中526.3/355.1和824.5/205.1分别用于M_1和S_1的外标法定量。维吉尼亚霉素M_1和S_1在1.0μg/kg^1 000.0μg/kg范围内线性关系良好,相关系数为0.998 7~0.999 5,添加饲料中添加水平为2.0、5.0、10.0μg/kg时,回收率在81.0%~105.0%之间,相对标准偏差(RSD)均小于4.0%(n=6),最低检出限和定量限分别为1.0μg/kg和2.0μg/kg。实验结果表明,该方法准确度高,省时,操作简单,成本低,重现性好,结果可靠,实用性强。A high performance liquid chromatography-tandem mass spectrometric （HPLC-MS/MS）method was developed for the determination of virginiamycin （VGM） M1 and S1 residues in feeds. The samples were extracted with acetonitrile, purified by freezing de-fatted and salting-out effect of saturated sodium chloride solution and redissolved in methanol-ammonium formate solution. The extracts were separated with XDB-C8 LC column using a binary eluent under gradient elution and determined by tandem mass spectrometry under positive electrospray ionization mode with multiple reaction monitoring （MRM） mode. m/z M1：526.3/355.1 and 526.3/337.2,S1：824.5/290.1 and 824.5/205.1 were selected as precursor-product ion pairs, in which 526.3/355.1 and 824.5/205.1 were used for external standard quantization. Under the optimal conditions , the calibration curve was linear over the concentration of VGM in the range of 1.0 μg/kg-1 000.0 μg/kg with correlation coefficient between 0.998 7-0.999 5. The quantitation limit of 2.0μg/kg and the detection limit was 1.0μg/kg. The average fortified recoveries of VGM from feeds at 3 spiked levels of 2.0 , 5.0 and 10μg/kg ranged from 81.0%to 105.0%with relative standard deviations（RSD）（n=6） less than 4.0%. The method showed good simplicity, sensitivity, stability, accuracy, time saving and low cost, and was suitable for the rapid determination of VGM in feedstuffs.

关 键 词：维吉尼亚霉素M_1和S_1 高效液相色谱-质谱/质谱 乙腈提取 冷冻脱脂 盐析净化 饲料 快速测定 

分 类 号：O657.63[理学—分析化学] S816.17[理学—化学]