A rapid, sensitive and specific ultra-high-performance liquid chromatography tandem mass spectrometry （UPLC-MS） method was developed for the analysis of tetracycline antibiotics, including tetracycline （TC）, oxyte...A rapid, sensitive and specific ultra-high-performance liquid chromatography tandem mass spectrometry （UPLC-MS） method was developed for the analysis of tetracycline antibiotics, including tetracycline （TC）, oxytetracycline （OTC）, chlortetracycline （CTC） and their 4-epimers （4-epiTCs） in agricultural soil fertilized with swine manure. Soil samples were extracted and cleaned-up with 10 mL EDTA-McIlvaine buffer solution （pH 4.0）, then cleaned-up and pre-concentrated using the Oasis MAX cartridge and then eluted with 1 mL solution by mixing formic acid, methanol and water at a ratio of 2：15：83 （v/v/v）. The purified samples were separated by an ACQUITY UPLC BEH C18 column using acetonitrile and water containing 0.1% formic acid mobile phase and detected by a single quadrupole MS. The limits of detection for the soil extraction method （LODsoil） ranged from 0.6-2.5 lag kg-~ with recoveries from 23.3-159.2%. Finally, the method was applied to an agricultural field in an area with intensive pig-fattening farming. Tetracyclines were detected in soil from 2.8 to 42.4 μg kg-1 soil. These results demonstrate that soil from swine farms can become severely contaminated with tetracycline antibiotics and their metabolites.展开更多
Quality control and screening of active substances in traditional Chinese medicines have been performed using fingerprint analysis. The spectrum-effect relationship between chromatography fingerprints and efficacy of ...Quality control and screening of active substances in traditional Chinese medicines have been performed using fingerprint analysis. The spectrum-effect relationship between chromatography fingerprints and efficacy of herbal drugs is considered as a potentially useful method for determining active ingredients in complex mixtures. The study was designed to develop a method for determining the bioactive components of a compound Chinese medicine called Tiefeng based on spectrum-effect relationships between high-performance liquid chromatography （HPLC） fingerprints and anticoccidial activities. Four peaks of the established HPLC fingerprint indicate the main bioactive components of this medicine. In addition, pharrnacodynamic atlas was defined and used to assess the anticoccidial activity of Tiefeng from different sources for the first time. We found that the level of anticoccidial activity of Tiefeng was consistent with the degree of similarity between the pharmacodynamic atlas and chromatogram of any sample. Furthermore, effect of this medicine was related with the main active constituents, along with the origin and the harvesting time.展开更多
Ethanamizuril(EZL) is a novel triazine anticoccidial compound that has high anticoccidial activity in chickens. In order to treat coccidiosis rationally in poultry, a detection method was developed for ethanamizuril i...Ethanamizuril(EZL) is a novel triazine anticoccidial compound that has high anticoccidial activity in chickens. In order to treat coccidiosis rationally in poultry, a detection method was developed for ethanamizuril in broiler plasma, and then the pharmacokinetics studies were performed in broilers after oral administration of different dose levels. Ethanamizuril was administered as single oral doses at low(0.67 mg kgBW), medium(1.33 mg kgBW) and high(6.67 mg kgBW) levels in which the medium dose was that recommended in clinics. Plasma concentrations of ethanamizuril were determined using ultra-high performance liquid chromatography and the data were analyzed with a non-compartmental model. Peak plasma concentrations of ethanamizuril were(2.16±0.57),(3.91±0.71), and(23.71±5.02) mg Lat(5.17±1.80),(4.60±2.12), and(4.60±2.12) h, respectively. The terminal elimination half-lives(t) for ethanamizuril were(10.84±2.59),(10.66±2.47), and(13.34±3.10) h after oral administration at low, medium and high doses, respectively. The areas under the concentrationtime curve(AUC)) were(37.68±6.87),(73.19±9.18), and(485.76±125.10) mg Lh with mean residence times(MRT) of(14.79±3.03),(15.57±3.69), and(20.22±4.01) h at the 3 dosages, respectively. Ethanamizuril was absorbed rapidly and eliminated slowly. A comparison across the dose range indicated that the time to reach peak plasma concentration(T) values were similar while peak plasma concentration(C) and AUCwere positively correlated with increasing dosages. This study of the pharmacokinetics of an ethanamizuril solution in chickens provides a theoretical basis for the rational use in the clinic.展开更多
An Sb delta doping layer in silicon is grown at the temperature of 300℃ by silicon molecular beam epitaxy and characterized by the small angle x-ray reflectivity measurement using synchrotron radiation beam.The oscil...An Sb delta doping layer in silicon is grown at the temperature of 300℃ by silicon molecular beam epitaxy and characterized by the small angle x-ray reflectivity measurement using synchrotron radiation beam.The oscillations of the reflectivity caused by dopant Sb at Q as large as 14.5 are detected.Simulation of this curve as a whole shows that the total amount of dopant Sb is 0.15 monolayer and is restricted to two atomic layers.An extremely narrow Sb delta doping structure without Sb segregation is thus obtained at the growth temperature of 300℃ as verified by the experiment.展开更多
文摘A rapid, sensitive and specific ultra-high-performance liquid chromatography tandem mass spectrometry （UPLC-MS） method was developed for the analysis of tetracycline antibiotics, including tetracycline （TC）, oxytetracycline （OTC）, chlortetracycline （CTC） and their 4-epimers （4-epiTCs） in agricultural soil fertilized with swine manure. Soil samples were extracted and cleaned-up with 10 mL EDTA-McIlvaine buffer solution （pH 4.0）, then cleaned-up and pre-concentrated using the Oasis MAX cartridge and then eluted with 1 mL solution by mixing formic acid, methanol and water at a ratio of 2：15：83 （v/v/v）. The purified samples were separated by an ACQUITY UPLC BEH C18 column using acetonitrile and water containing 0.1% formic acid mobile phase and detected by a single quadrupole MS. The limits of detection for the soil extraction method （LODsoil） ranged from 0.6-2.5 lag kg-~ with recoveries from 23.3-159.2%. Finally, the method was applied to an agricultural field in an area with intensive pig-fattening farming. Tetracyclines were detected in soil from 2.8 to 42.4 μg kg-1 soil. These results demonstrate that soil from swine farms can become severely contaminated with tetracycline antibiotics and their metabolites.
基金funded by the National Key Technology R&D Program, China (2008 BADB4B05-02)
文摘Quality control and screening of active substances in traditional Chinese medicines have been performed using fingerprint analysis. The spectrum-effect relationship between chromatography fingerprints and efficacy of herbal drugs is considered as a potentially useful method for determining active ingredients in complex mixtures. The study was designed to develop a method for determining the bioactive components of a compound Chinese medicine called Tiefeng based on spectrum-effect relationships between high-performance liquid chromatography （HPLC） fingerprints and anticoccidial activities. Four peaks of the established HPLC fingerprint indicate the main bioactive components of this medicine. In addition, pharrnacodynamic atlas was defined and used to assess the anticoccidial activity of Tiefeng from different sources for the first time. We found that the level of anticoccidial activity of Tiefeng was consistent with the degree of similarity between the pharmacodynamic atlas and chromatogram of any sample. Furthermore, effect of this medicine was related with the main active constituents, along with the origin and the harvesting time.
基金supported by the National Natural Science Foundation of China (31472235 and 31272607)the Natural Science Foundation of Shanghai, China (14ZR1449000)+2 种基金the Special Scientific Research Fund of Agricultural Public Welfare Profession of China (201303038)the Central Grade Public Welfare Fundamental Science Fund For Scientific Research Institute, China (2016JB08 and 2016JB04)the National Key Technology Research and Development Program of the Ministry of Science and Technology of China (2015BAD11B01-06)
文摘Ethanamizuril(EZL) is a novel triazine anticoccidial compound that has high anticoccidial activity in chickens. In order to treat coccidiosis rationally in poultry, a detection method was developed for ethanamizuril in broiler plasma, and then the pharmacokinetics studies were performed in broilers after oral administration of different dose levels. Ethanamizuril was administered as single oral doses at low(0.67 mg kgBW), medium(1.33 mg kgBW) and high(6.67 mg kgBW) levels in which the medium dose was that recommended in clinics. Plasma concentrations of ethanamizuril were determined using ultra-high performance liquid chromatography and the data were analyzed with a non-compartmental model. Peak plasma concentrations of ethanamizuril were(2.16±0.57),(3.91±0.71), and(23.71±5.02) mg Lat(5.17±1.80),(4.60±2.12), and(4.60±2.12) h, respectively. The terminal elimination half-lives(t) for ethanamizuril were(10.84±2.59),(10.66±2.47), and(13.34±3.10) h after oral administration at low, medium and high doses, respectively. The areas under the concentrationtime curve(AUC)) were(37.68±6.87),(73.19±9.18), and(485.76±125.10) mg Lh with mean residence times(MRT) of(14.79±3.03),(15.57±3.69), and(20.22±4.01) h at the 3 dosages, respectively. Ethanamizuril was absorbed rapidly and eliminated slowly. A comparison across the dose range indicated that the time to reach peak plasma concentration(T) values were similar while peak plasma concentration(C) and AUCwere positively correlated with increasing dosages. This study of the pharmacokinetics of an ethanamizuril solution in chickens provides a theoretical basis for the rational use in the clinic.
基金Supported by the National Natural Science Foundation of China under Grant No.69476008the Key Project of the State Commission of Science and Technology of China.
文摘An Sb delta doping layer in silicon is grown at the temperature of 300℃ by silicon molecular beam epitaxy and characterized by the small angle x-ray reflectivity measurement using synchrotron radiation beam.The oscillations of the reflectivity caused by dopant Sb at Q as large as 14.5 are detected.Simulation of this curve as a whole shows that the total amount of dopant Sb is 0.15 monolayer and is restricted to two atomic layers.An extremely narrow Sb delta doping structure without Sb segregation is thus obtained at the growth temperature of 300℃ as verified by the experiment.
