超高效液相色谱-串联质谱法测定饲料中的维吉尼霉素M_1  

Determination of virginiamycin M_1 in feeds by ultra high performance liquid chromatography-tandem mass spectrometry

作　　者：黄永辉 

机构地区：[1]福建省产品质量检验研究院,国家加工食品质量监督检验中心,福建福州350002

出　　处：《色谱》2011年第10期962-966,共5页Chinese Journal of Chromatography

基　　金：福建省质量技术监督局科技计划项目(FJQI2009018)

摘　　要：建立了饲料中维吉尼霉素M1的超高效液相色谱-串联质谱(UPLC-MS/MS)分析测定方法。样品用乙腈-0.2%(v/v)甲酸水溶液(8∶2,v/v)超声提取两遍后,通过UPLC-MS/MS进行分析,以BEH C18色谱柱为分析柱,乙腈-0.3%(v/v)甲酸水溶液(35∶65,v/v)为流动相,采用电喷雾电离正离子模式,以多反应监测模式进行定性和定量分析。在0.3～226.6μg/L范围内线性关系良好(相关系数r=0.999 5)。维吉尼霉素M1的检出限和定量限分别为2μg/kg和7μg/kg,平均回收率为82.6%～102.7%,相对标准偏差为0.9%～10.5%。结果表明,该方法具有操作简单、准确度和灵敏度高、重现性好的特点,适合用于检测饲料中维吉尼霉素M1的含量。A comprehensive analytical method based on ultra high performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS） has been developed for the determination of virginiamycin M1 in feeds.The sample was extracted twice by ultrasonic extraction with acetonitrile-0.2%（v/v） formic acid（8∶2,v/v）.The chromatographic separation was achieved with a BEH C18 column and acetonitrile-0.3%（v/v） formic acid（35∶65,v/v） as the mobile phase.The identification and quantification of the analyte were carried out on electrospray ionization MS/MS in a multiple reaction monitoring（MRM） mode.The correlation coefficient（r） of virginiamycin M1 was 0.999 5 in the linear range of 0.3-226.6 μg/L.The detection limit（S/N=3） and quantification limit（S/N=10） of virginiamycin M1 were 2 μg/kg and 7 μg/kg,respectively.The average spiked recoveries were in the range of 82.6% to 102.7% with the relative standard deviations（RSDs） of 0.9%-10.5%.The results demonstrate that the proposed method is simple,sensitive,repeatable and suitable for the testing of virginiamycin M1 in feeds.

关 键 词：超高效液相色谱-串联质谱 维吉尼霉素M1 饲料 

分 类 号：O658[理学—分析化学]