摘要
建立了凝胶渗透色谱-固相萃取/高效液相色谱法测定水产品中甲基睾酮和己烯雌酚的分析方法。样品经乙醚超声提取和漩涡振荡后以乙酸乙酯-环己烷(1∶1)为流动相进行凝胶渗透色谱净化,再过HLB柱进一步净化,以甲醇-水(72∶28)为流动相,采用高效液相色谱/紫外检测器在254 nm波长下测定,外标法定量。结果显示甲基睾酮和己烯雌酚在0.02~2.0 mg/L质量浓度范围内呈良好的线性关系,线性系数(r)均大于0.999。空白样品在10.0、50.0、200μg/kg 3个加标水平下的平均回收率为84%~93%,相对标准偏差均小于6.0%。甲基睾酮和己烯雌酚的定量下限分别为6.0μg/kg和5.0μg/kg。
A method of high performance liquid chromatography combined with gel permeation chro- matography(GPC/HPLC) was developed for the simultaneous analysis of methyhestosterone (MET) and diethylstilbestrol(DES) in aquatic products. The homogenized samples were extracted with dieth- yl ether, then cleaned by GPC using ethyl acetate -cyclohexane( 1 : 1 )as mobile phase, follwed by a further HLB solid phase extraction. The targeted compounds were detected by HPLC - ultraviolet detector at the wavelength of 254 nm, using methanol -water(72 : 28) as mobile phase, and quan- tified by the external standard method. The calibration curves of two compounds were linear in the concentration range of 0. 02 - 2. 0 mg/L with correlation coefficients more than 0. 999. The average recoveries of MET and DES at spiked concentrations of 10. 0, 50. 0, 200 μg/kg ranged from 84% to 93% , with relative standard deviations(RSDs) less than 6. 0%. The LOQs of MET and DES were 6. 0 μg/kg and 5.0 μg/kg, respectively.
出处
《分析测试学报》
CAS
CSCD
北大核心
2013年第2期267-270,共4页
Journal of Instrumental 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)
关键词
凝胶渗透色谱
固相萃取
高效液相色谱
水产品
甲基睾酮
己烯雌酚
gel permeation chromatography ( GPC )
solid phase extraction ( SPE )
high performance liquid chromatography ( HPLC )
aquatic products
methyltestosterone (MET)
diethylstilbestrol ( DES )