超高效液相色谱-串联质谱法测定饲料中的维吉尼霉素M1

摘要

A comprehensive analytical method based on ultra high performance liquid chroma-tography-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 ace-tonitrile-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 ioni-zation MS/MS in a multiple reaction monitoring (MKM) mode. The correlation coefficient (r) of virginiamycin M, 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 M, 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.%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 3～226.6 μg/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2 μg/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.