建立了黄油中雌酮、α-雌二醇、β-雌二醇、雌三醇、睾酮、表睾酮、孕酮和丙酸睾酮8种类固醇激素的凝胶渗透色谱(GPC)-液相色谱/串联质谱(LC-MS/MS)检测方法。样品用乙酸乙酯-环己烷(1∶1,V/V)提取,提取液经GPC柱净化除脂,GPC浓缩液采用C18色谱柱(100 mm×2.0 mm i.d.,3.0μm)分离,以乙腈和水为流动相进行梯度洗脱,电喷雾电离多反应监测模式进行定性和定量分析。8种类固醇激素以基质匹配外标法定量,药物在1.0~20.0μg/kg线性范围内相关系数(r)均大于0.999;方法检出限(S/N=3)为0.04~0.30μg/kg,定量限LOQs(S/N=10)为1.0μg/kg;添加水平为1.0,2.0,4.0μg/kg时,回收率范围在64.1%~110%之间;相对标准偏差(RSD)小于11%。结果表明,本方法准确、可靠,满足黄油中8种类固醇激素的检测分析要求。 相似文献
Sediment-water interfaces are important interfaces for lakes, which are related to most environmental and ecological problems. Wind-induced waves cause secondary pollution via sediment resuspension. Since the coupling mechanism of water, resuspended sediments, and phosphorus affects the release of phosphorus (P) near the interface, a coupled model was explored for two sediment types with different adsorption-desorption capabilities to examine sediment resuspension and P release. The relationships among wind speed, wave characteristics, sediment distribution and P concentration were obtained. For different sediments, the unit sediment desorption release is negatively correlated with wind speed. When sediments are resuspended under low or moderate wind speed, the P concentration in the overlying water increases abruptly, hampering diffusion. P release exhibits the characteristics of concentrated release in a small region and changes the water environment rapidly.