摘要
提出了水产品中甲基睾酮的超高效液相色谱-串联质谱法分析方法。样品经叔丁基甲醚提取,提取液经凝胶渗透色谱和HLB固相萃取柱净化,所得洗脱液40℃氮吹挥干后用流动相溶解,用ACQUITY UPLC BEH C18色谱柱分离,以乙腈-0.2%甲酸(40+60)溶液为流动相洗脱,采用电喷雾正离子源及多反应监测模式测定。甲基睾酮的质量浓度在0.50～100μg.L-1范围内呈线性关系,测定下限(10S/N)为0.5μg.kg-1。添加1.0,5.0,10.0μg.kg-1 3个浓度水平进行加标回收试验,回收率在87.0%～94.2%之间,测定值的相对标准偏差(n=5)均小于6%。
A method for the determination of 17a-methyltestosterone （MET） in aquatic products by UHPLC- MS/MS was proposed. The sample was extracted with tert-butyl methyl ether, and the extract obtained was purified by gel permeation chromatography atld HLB SPE column. Eluate from the column was evaporated to near dryness by N2-blowing at 40 ℃, and the residue was dissolved with the mobile phase mixture. ACQUITY UPLC lgEH C18 column was used as chromatographic column, and a mixture of acetonitrile and 0. 2% formic acid （40＋60） was used as mobile phase in gradient eiution; positive eleetrospray ionization and multiple reactions monitoring mode were used in the detection. Linearity range for MET was kept between 0. 50- 100 μg·g^-1 , with lower limit of determination （10S/N） of 0. 5 μg·g^-1 Tests for recovery were made at the concentration levels of 1.0, 5.0, 10. 0 μg·g^-1 of standard MET, giving values of recovery in the range of 87. 0%--94. 2%, with RSDrs （n=5） less than 6%.
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2013年第5期570-572,576,共4页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
浙江省科技计划项目(2012F30021)
浙江省重点科技创新团队项目(2010R50028)
