为模拟人体表面温度和酸度，用人工酸性汗液提取样品，用氢化反应一原子荧光法对提取汗液中的砷进行测定，优化了氢化反应条件，并给出合适的荧光光谱分析参数，建立了灵敏度高、干扰少、操作简便、成本较低的砷的检测方法；测试结果表...为模拟人体表面温度和酸度，用人工酸性汗液提取样品，用氢化反应一原子荧光法对提取汗液中的砷进行测定，优化了氢化反应条件，并给出合适的荧光光谱分析参数，建立了灵敏度高、干扰少、操作简便、成本较低的砷的检测方法；测试结果表明，该方法的检出低限为0．026mg／kg，可满足Oeko-Tex Standard 100对纺织品中可萃取砷0．2mg／kg的限量要求。选取多种纺织纤维，进行标准添加回收实验，回收率在82％～105％之间，标准偏差(RSD)小于10％。展开更多
A determination method has been optimized and validated for the simultaneous analysis of tetracycline （TC）, oxytetracycline （OTC）, chlortetracycline （CTC） and doxycycline （DC） in honey. Tetracyclines （TCs） w...A determination method has been optimized and validated for the simultaneous analysis of tetracycline （TC）, oxytetracycline （OTC）, chlortetracycline （CTC） and doxycycline （DC） in honey. Tetracyclines （TCs） were removed from honey samples by chelation with metal ions bound to small Chelating Sepharose Fast Flow columns and eluted with Na2EDTA-Mcllvaine pH 4.0 buffers. Extracts were further cleaned up by Oasis HLB solid-phase extraction （SPE）, while other solid-phase extraction cartridges were compared. Chromatographic separation was achieved using a polar end-capped C 18 column with an isocratic mobile phase consisting of oxalic acid, acetonitrile and methanol. LC with ultraviolet absorbance at 355 nm resulted in the quantitation of all four tetracycline residues from honey samples fortified at 15, 50, and 100 ng/g, with liner ranges for tetracyclines of 0.05 to 2 μg/mL. Mean recoveries for tetracyclines were greater than 50% with R.S.D. values less than 10% （n= 18）. Detection limits of 5, 5, 10, 10 ng/g for oxytetracycline, tetracycline, chlortetracycline and doxycycline, respectively and quantitation limits of 15 ng/g for all the four tetracyclines were determined. Direct confirmation of the four residues in honey （2-50 ng/g） was realized by liquid chromatography-tandem mass spectrometry （LC/MS/MS）. The linear ranges of tetracyclines determined by LC/MS/MS were between 5 to 300 ng/mL, with the linear correlation coefficient r〉 0.995. The limits of detection of 1 to 2 ng/g were obtained for the analysis of the TCs in honey.展开更多
文摘为模拟人体表面温度和酸度，用人工酸性汗液提取样品，用氢化反应一原子荧光法对提取汗液中的砷进行测定，优化了氢化反应条件，并给出合适的荧光光谱分析参数，建立了灵敏度高、干扰少、操作简便、成本较低的砷的检测方法；测试结果表明，该方法的检出低限为0．026mg／kg，可满足Oeko-Tex Standard 100对纺织品中可萃取砷0．2mg／kg的限量要求。选取多种纺织纤维，进行标准添加回收实验，回收率在82％～105％之间，标准偏差(RSD)小于10％。
文摘A determination method has been optimized and validated for the simultaneous analysis of tetracycline （TC）, oxytetracycline （OTC）, chlortetracycline （CTC） and doxycycline （DC） in honey. Tetracyclines （TCs） were removed from honey samples by chelation with metal ions bound to small Chelating Sepharose Fast Flow columns and eluted with Na2EDTA-Mcllvaine pH 4.0 buffers. Extracts were further cleaned up by Oasis HLB solid-phase extraction （SPE）, while other solid-phase extraction cartridges were compared. Chromatographic separation was achieved using a polar end-capped C 18 column with an isocratic mobile phase consisting of oxalic acid, acetonitrile and methanol. LC with ultraviolet absorbance at 355 nm resulted in the quantitation of all four tetracycline residues from honey samples fortified at 15, 50, and 100 ng/g, with liner ranges for tetracyclines of 0.05 to 2 μg/mL. Mean recoveries for tetracyclines were greater than 50% with R.S.D. values less than 10% （n= 18）. Detection limits of 5, 5, 10, 10 ng/g for oxytetracycline, tetracycline, chlortetracycline and doxycycline, respectively and quantitation limits of 15 ng/g for all the four tetracyclines were determined. Direct confirmation of the four residues in honey （2-50 ng/g） was realized by liquid chromatography-tandem mass spectrometry （LC/MS/MS）. The linear ranges of tetracyclines determined by LC/MS/MS were between 5 to 300 ng/mL, with the linear correlation coefficient r〉 0.995. The limits of detection of 1 to 2 ng/g were obtained for the analysis of the TCs in honey.
