建立了液相色谱-四极杆/静电场轨道阱高分辨质谱法监测口服液中33种芬太尼类精神药物的定向自动筛查方法。样品在盐析的作用下,乙腈超声提取,固相基质分散净化,在电喷雾正离子模式下,一级四极杆质谱在m/z 2.0隔离窗口下过滤带电分子离子...建立了液相色谱-四极杆/静电场轨道阱高分辨质谱法监测口服液中33种芬太尼类精神药物的定向自动筛查方法。样品在盐析的作用下,乙腈超声提取,固相基质分散净化,在电喷雾正离子模式下,一级四极杆质谱在m/z 2.0隔离窗口下过滤带电分子离子,高分辨静电场轨道阱质谱自动触发子离子全扫描分析,根据芬太尼的精确质量数、同位素丰度比、二级碎片离子建立标准物质数据库,采用Trace Finder 5.1软件自动检索匹配完成目标物的筛查。口服液中33种芬太尼类方法定量限为(LOQ)10μg/kg,分析物在5~200μg/kg浓度范围内线性关系良好,相关系数R^(2)≥0.9993;方法回收率在72.6%~102.4%之间,相对标准偏差为3.8%~10.5%。结果表明,所建立的筛查方法可用于口服液中33种芬太尼类精神药物的自动筛查与测定,具有准确、快速、实用的特点。展开更多
Studies of Daphnia distribution and function could help people manage and protect water quality. We investigated how spatial distribution and filtering efficiency of Daphnia in the transition and lacustrine zones of t...Studies of Daphnia distribution and function could help people manage and protect water quality. We investigated how spatial distribution and filtering efficiency of Daphnia in the transition and lacustrine zones of the Nanwan Reservoir (China). Samplings were conducted seasonally for 2 years from six sites in the reservoir. Daphnia abundance and biomass were significantly higher in the lacustrine zone than in the transition zone. Similar composition and biomass of edible phytoplankton were found in the two zones, suggesting that food quantity could not explain high Daphnia distribution in the lacustrine zone. The variations of water velocity and food quality could help explaining Daphnia patchy distribution in the reservoir. On the one hand, rapid water velocity can cause the Daphnia decrement in the transition zone. On the other hand, the ratio of particulate organic carbon (POC) to chlorophyll a (chl a) concentration was significantly higher in the transition zone, indicating more allochthonous material constituted the food source for Daphnia. The lower quality food likely suppressed Daphnia development in the transition zone. A linear regression between Daphnia abundance and Secchi depth (SD) may suggest a cause-effect relationship where increased filtering efficiency was responsible for increased water clarity to some extent.展开更多
采用气相色谱-稳定同位素比值质谱(Gas chromatography-stable isotope ratio mass spectrometry,GC-IRMS)技术测定三文鱼中16种氨基酸碳同位素δ13C值分布。以16种特征氨基酸为溯源分析对象,首先采用盐酸水解蛋白,再进行甲酯和乙酰化...采用气相色谱-稳定同位素比值质谱(Gas chromatography-stable isotope ratio mass spectrometry,GC-IRMS)技术测定三文鱼中16种氨基酸碳同位素δ13C值分布。以16种特征氨基酸为溯源分析对象,首先采用盐酸水解蛋白,再进行甲酯和乙酰化衍生反应,生成的衍生物用35%苯基-甲基聚硅氧烷色谱柱分离。在优化的GC-IRMS试验参数下,16种氨基酸方法检出限为50 mg/kg,质控品谷氨基酸在不同批次间标准偏差为0.84%。经对来自挪威、法罗群岛、澳大利亚、智利、美国、新西兰这6个产地的三文鱼进行测定,测得三文鱼δ^(13)C值在–3.116%至–0.165%之间,标准偏差(n=5)≤4.2%。通过获得不同产地三文鱼中16种特征功能性氨基酸指纹图谱,分析了三文鱼中不同特征氨基酸功能成分间δ^(13)C值的相关性,并对每种氨基酸对产地、养殖方式溯源因子鉴定的贡献进行了分析。在统计分析的基础上,完成不同产地、不同生长方式三文鱼的溯源鉴定模型。对实际样品进行测定,证明三文鱼体内蛋白氨基酸成分可作为特征指标,可用于对三文鱼进行产地、养殖方式进行溯源鉴别,测定结果可靠。展开更多
Novel tentacle-type chiral adsorbent based on silica gels modified with β-cyclodextrin (β-CD) and polyvinyl alcohol(PVA) is synthesized by surface grafting technique. The adsorption behavior of chiral pharmaceutical...Novel tentacle-type chiral adsorbent based on silica gels modified with β-cyclodextrin (β-CD) and polyvinyl alcohol(PVA) is synthesized by surface grafting technique. The adsorption behavior of chiral pharmaceuticals using the resulting adsorbents is investigated. In the study, FT-IR and thermogravimetric analysis (TGA) are employed to characterize the chemical and physical properties of the adsorbent; mandelic acid (MA) serves as model solute to evaluate the sorption capacity and selectivity of the adsorbent. The experimental results show that the novel tentacle-type adsorbent is possessed of larger equilibrium adsorption capacity and better selectivity over the conventional one and could be as potential chiral stationary phase (CSPs).展开更多
文摘建立了液相色谱-四极杆/静电场轨道阱高分辨质谱法监测口服液中33种芬太尼类精神药物的定向自动筛查方法。样品在盐析的作用下,乙腈超声提取,固相基质分散净化,在电喷雾正离子模式下,一级四极杆质谱在m/z 2.0隔离窗口下过滤带电分子离子,高分辨静电场轨道阱质谱自动触发子离子全扫描分析,根据芬太尼的精确质量数、同位素丰度比、二级碎片离子建立标准物质数据库,采用Trace Finder 5.1软件自动检索匹配完成目标物的筛查。口服液中33种芬太尼类方法定量限为(LOQ)10μg/kg,分析物在5~200μg/kg浓度范围内线性关系良好,相关系数R^(2)≥0.9993;方法回收率在72.6%~102.4%之间,相对标准偏差为3.8%~10.5%。结果表明,所建立的筛查方法可用于口服液中33种芬太尼类精神药物的自动筛查与测定,具有准确、快速、实用的特点。
基金Supported by the National Natural Science Foundation of China(Nos.31400397,31700405)the Foundation of He’nan Science and Technology Department(No.172102210345)
文摘Studies of Daphnia distribution and function could help people manage and protect water quality. We investigated how spatial distribution and filtering efficiency of Daphnia in the transition and lacustrine zones of the Nanwan Reservoir (China). Samplings were conducted seasonally for 2 years from six sites in the reservoir. Daphnia abundance and biomass were significantly higher in the lacustrine zone than in the transition zone. Similar composition and biomass of edible phytoplankton were found in the two zones, suggesting that food quantity could not explain high Daphnia distribution in the lacustrine zone. The variations of water velocity and food quality could help explaining Daphnia patchy distribution in the reservoir. On the one hand, rapid water velocity can cause the Daphnia decrement in the transition zone. On the other hand, the ratio of particulate organic carbon (POC) to chlorophyll a (chl a) concentration was significantly higher in the transition zone, indicating more allochthonous material constituted the food source for Daphnia. The lower quality food likely suppressed Daphnia development in the transition zone. A linear regression between Daphnia abundance and Secchi depth (SD) may suggest a cause-effect relationship where increased filtering efficiency was responsible for increased water clarity to some extent.
文摘采用气相色谱-稳定同位素比值质谱(Gas chromatography-stable isotope ratio mass spectrometry,GC-IRMS)技术测定三文鱼中16种氨基酸碳同位素δ13C值分布。以16种特征氨基酸为溯源分析对象,首先采用盐酸水解蛋白,再进行甲酯和乙酰化衍生反应,生成的衍生物用35%苯基-甲基聚硅氧烷色谱柱分离。在优化的GC-IRMS试验参数下,16种氨基酸方法检出限为50 mg/kg,质控品谷氨基酸在不同批次间标准偏差为0.84%。经对来自挪威、法罗群岛、澳大利亚、智利、美国、新西兰这6个产地的三文鱼进行测定,测得三文鱼δ^(13)C值在–3.116%至–0.165%之间,标准偏差(n=5)≤4.2%。通过获得不同产地三文鱼中16种特征功能性氨基酸指纹图谱,分析了三文鱼中不同特征氨基酸功能成分间δ^(13)C值的相关性,并对每种氨基酸对产地、养殖方式溯源因子鉴定的贡献进行了分析。在统计分析的基础上,完成不同产地、不同生长方式三文鱼的溯源鉴定模型。对实际样品进行测定,证明三文鱼体内蛋白氨基酸成分可作为特征指标,可用于对三文鱼进行产地、养殖方式进行溯源鉴别,测定结果可靠。
基金supported by the Doctoral Fund of Ministry of Education of China (20090181110043)
文摘Novel tentacle-type chiral adsorbent based on silica gels modified with β-cyclodextrin (β-CD) and polyvinyl alcohol(PVA) is synthesized by surface grafting technique. The adsorption behavior of chiral pharmaceuticals using the resulting adsorbents is investigated. In the study, FT-IR and thermogravimetric analysis (TGA) are employed to characterize the chemical and physical properties of the adsorbent; mandelic acid (MA) serves as model solute to evaluate the sorption capacity and selectivity of the adsorbent. The experimental results show that the novel tentacle-type adsorbent is possessed of larger equilibrium adsorption capacity and better selectivity over the conventional one and could be as potential chiral stationary phase (CSPs).
