A highly sensitive method was developed for the simultaneous determination of 8 steroid hormones in high-fat fish tissues using ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The 8 s...A highly sensitive method was developed for the simultaneous determination of 8 steroid hormones in high-fat fish tissues using ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The 8 steroid hormones were extracted from the tissues with diethyl ether.Differing from other common purification methods,the extract solutions were cleaned by gel permeation chromatography(GPC) using ethyl acetate-cyclohexane solution(1:1,v/v) as the mobile phase.The separation of target compounds was carried out by a BEH C18 column and a gradient elution consisting of acetonitrile and 0.2% aqueous formic acid(v/v).The compounds were detected under the multiple reaction monitoring(MRM) mode and quantified with external standard method.This method was validated with respect to linearity,specificity,accuracy and precision.A linearity with correlation coefficient larger than 0.995 was achieved in the range of 0.5 to 50 ng m L^(-1).The average recoveries at the spiked levels of 1.0,5.0,and 10.0 μg kg^(–1) varied between 81.7% and 90.8%,with the relative standard deviations(n=5) ranged from 3.50% to 10.0%.The limit of quantification(LOQ) for 8 steroid hormones ranged from 0.2 to 1.5 μg kg^(-1).It was concluded that this method can be successfully applied for the determination of 8 steroid hormones in complicated matrices including high-fat fish tissues.展开更多
目的建立一种在线凝胶色谱-气相色谱-质谱(gel permeation chromatography coupled with gas chromatography-mass spectrometry,GPC-GC/MS)联用法测定淡水鱼中农药残留的检测方法。方法采用超声辅助技术和高效萃取吸管法对南昌地区淡...目的建立一种在线凝胶色谱-气相色谱-质谱(gel permeation chromatography coupled with gas chromatography-mass spectrometry,GPC-GC/MS)联用法测定淡水鱼中农药残留的检测方法。方法采用超声辅助技术和高效萃取吸管法对南昌地区淡水鱼样品净化处理,以乙腈为提取液,采用氯化钠去除水分后,经在线GPC-GC-MS系统进样分析,选择离子检测方式定量检测。结果25种化合物的质量浓度在一定范围内与其对应的峰面积有良好的线性关系,相关系数大于0.996,方法的检出限为9.1×10^-5-3.1×10^-1mg/kg。以空白样品为基体进行加标回收实验,回收率为71.4%~103.2%,相对标准偏差小于9%。结论该方法前处理简单快速,灵敏度高,有机溶剂使用量少,适用于淡水鱼中农药残留的检测。展开更多
基金supported by the Natural Science Foundation of Zhejiang Province,China(No.LY17C200009)the Foundation of Zhejiang Educational Committee(No.Y201328477)
文摘A highly sensitive method was developed for the simultaneous determination of 8 steroid hormones in high-fat fish tissues using ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The 8 steroid hormones were extracted from the tissues with diethyl ether.Differing from other common purification methods,the extract solutions were cleaned by gel permeation chromatography(GPC) using ethyl acetate-cyclohexane solution(1:1,v/v) as the mobile phase.The separation of target compounds was carried out by a BEH C18 column and a gradient elution consisting of acetonitrile and 0.2% aqueous formic acid(v/v).The compounds were detected under the multiple reaction monitoring(MRM) mode and quantified with external standard method.This method was validated with respect to linearity,specificity,accuracy and precision.A linearity with correlation coefficient larger than 0.995 was achieved in the range of 0.5 to 50 ng m L^(-1).The average recoveries at the spiked levels of 1.0,5.0,and 10.0 μg kg^(–1) varied between 81.7% and 90.8%,with the relative standard deviations(n=5) ranged from 3.50% to 10.0%.The limit of quantification(LOQ) for 8 steroid hormones ranged from 0.2 to 1.5 μg kg^(-1).It was concluded that this method can be successfully applied for the determination of 8 steroid hormones in complicated matrices including high-fat fish tissues.
文摘目的建立一种在线凝胶色谱-气相色谱-质谱(gel permeation chromatography coupled with gas chromatography-mass spectrometry,GPC-GC/MS)联用法测定淡水鱼中农药残留的检测方法。方法采用超声辅助技术和高效萃取吸管法对南昌地区淡水鱼样品净化处理,以乙腈为提取液,采用氯化钠去除水分后,经在线GPC-GC-MS系统进样分析,选择离子检测方式定量检测。结果25种化合物的质量浓度在一定范围内与其对应的峰面积有良好的线性关系,相关系数大于0.996,方法的检出限为9.1×10^-5-3.1×10^-1mg/kg。以空白样品为基体进行加标回收实验,回收率为71.4%~103.2%,相对标准偏差小于9%。结论该方法前处理简单快速,灵敏度高,有机溶剂使用量少,适用于淡水鱼中农药残留的检测。
